02834nas a2200253 4500008004100000022001400041245007900055210006900134260007100203300001400274490000700288520198600295653001402281653002002295653001302315653000802328653002602336653001802362100001902380700001902399700002702418700002202445856011302467 2013 eng d a0897-475600aLarge centimeter-sized macroporous ferritin gels as versatile nanoreactors0 aLarge centimetersized macroporous ferritin gels as versatile nan a1155 16TH ST, NW, WASHINGTON, DC 20036 USAbAMER CHEMICAL SOCcDEC a4813-48190 v253 a

Organized assemblies of bionanoparticles such as ferritin provides templates that can be exploited for nanotechnological applications. Organization of ferritin into well-defined three-dimensional assemblies is challenging and has attracted considerable attention recently. We have synthesized, for the first time, large (centimeter-sized) self-standing macroporous scaffold monoliths from ferritin bionanoparticles, using dynamic templating of surfactant H-1 domains. These scaffolds comprise three-dimensionally connected strands of ferritin, organized as a porous gel with porosity similar to 55 mu m. The iron oxide inside the ferritin scaffold can be easily replaced with catalytically active monodisperse zerovalent transition metal nanoparticles using a very simple protocol. Since the ferritin is cross-linked in the scaffold, it is significantly robust with enhanced thermal stability and better tolerance toward several organic solvents in Comparison to the native ferritin bionanoparticle. In addition, the scaffold macropores facilitate substrate and reagent transport and hence the monoliths containing active Pd or iron oxide nanoparticles inside apo-ferritin bionanoparticles were used as a recyclable heterogeneous catalyst for the oxidation of 2,3,6-trimethyl phenol to 2,3,6-trimethyl-1,4-benzoquinone (precursor for Vitamin E synthesis) and for Suzuki-Miyaura cross-coupling reaction in both aqueous and organic solvents. The protein shell around the nanoparticles protects them from agglomeration, a phenomenon that otherwise plagues nanoparticles-based catalysis. The presence of macropores allow the ferritin scaffold to act as catalytic monolith for continuous flow reactions having rapid reaction rates, while offering a low pressure drop. Finally, the Pd@apo-ferritin scaffold was immobilized inside a steel cartridge and used for the continuous flow hydrogenation of alkenes to their corresponding alkanes for 15 cycles without any loss of activity.

10acatalysis10acontinuous flow10aferritin10agel10amacroporous materials10aSelf-assembly1 aKumari, Sushma1 aKulkarni, Amol1 aKumaraswamy, Guruswamy1 aGupta, Sayam, Sen uhttps://library.ncl.res.in/content/large-centimeter-sized-macroporous-ferritin-gels-versatile-nanoreactors-001398nas a2200217 4500008004100000022001400041245005400055210005400109260008600163300001200249490000700261520069400268653002000962653001900982653001801001653001401019653001601033653002001049100002301069856008801092 2014 eng d a1860-539700aContinuous flow nitration in miniaturized devices0 aContinuous flow nitration in miniaturized devices aTRAKEHNER STRASSE 7-9, FRANKFURT AM MAIN, 60487, GERMANYbBEILSTEIN-INSTITUTcFEB a405-4240 v103 a

This review highlights the state of the art in the field of continuous flow nitration with miniaturized devices. Although nitration has been one of the oldest and most important unit reactions, the advent of miniaturized devices has paved the way for new opportunities to reconsider the conventional approach for exothermic and selectivity sensitive nitration reactions. Four different approaches to flow nitration with microreactors are presented herein and discussed in view of their advantages, limitations and applicability of the information towards scale-up. Selected recent patents that disclose scale-up methodologies for continuous flow nitration are also briefly reviewed.

10acontinuous flow10aflow chemistry10amicroreactors10anitration10anitric acid10aTubular reactor1 aKulkarni, Amol, A. uhttps://library.ncl.res.in/content/continuous-flow-nitration-miniaturized-devices-001751nas a2200241 4500008004100000022001400041245009300055210006900148260000900217300001400226490000800240520095100248653002501199653003001224653000801254653002001262653002601282653001901308100001501327700001801342700002301360856012601383 2019 eng d a1385-894700aAntisolvent based precipitation: batch, capillary flow reactor and impinging jet reactor0 aAntisolvent based precipitation batch capillary flow reactor and cAUG  a1161-11710 v3693 a

A method for continuous antisolvent precipitation of ammonium perchlorate (AP) using a confined impinging jet reactor (CIJR) is studied. The geometry of the CIJR was optimized to achieve excellent mixing with a significant reduction in the particle deposition on walls. Initially, the experimental conditions were optimized in a batch system and then in a continuous capillary reactor. Later those conditions extended for antisolvent precipitation of AP in an impinging jet reactor using water and n-butyl alcohol as a solvent and antisolvent, respectively for optimum performance. The performance was compared with the experiments in batch mode as well as and in a continuous capillary reactor. Over a range of inlet jet velocity that corresponded to 1792 < Re < 7193 for the saturated aqueous solution of AP and 1135 < Re < 4553 for the antisolvent butanol phase, 8.98-16.98 mu m Ammonium perchlorate particles were attained.

10aAmmonium perchlorate10aAntisolvent precipitation10aCFD10acontinuous flow10aImpinging jet reactor10amicroparticles1 aPal, Sayan1 aMadane, Ketan1 aKulkarni, Amol, A. uhttps://library.ncl.res.in/content/antisolvent-based-precipitation-batch-capillary-flow-reactor-and-impinging-jet-reactor01728nas a2200277 4500008004100000022001400041245009200055210006900147260000800216300001200224490000700236520085900243653002001102653001401122653001701136653000801153653001301161100002001174700002301194700001801217700002801235700001701263700002601280700002301306856012101329 2021 eng d a2062-249X00aDesign and scale-up of continuous di-nitration reaction using pinched tube flow reactor0 aDesign and scaleup of continuous dinitration reaction using pinc cSEP a611-6240 v113 aScale-up of the di-nitration reaction for synthesis of selective herbicide pendimethalin using only nitric acid in continuous flow is presented in this work. This work showcases an approach for smooth scale-up for an herbicide for a production capacity of 50 kg/day using a pinched tube reactor. The approach begins with the batch experiments followed by flow synthesis using a 1/8-inchSS316 helical coil tube where kinetics of the di-nitration was determined, and process optimization was done. Systematic approach was followed for quantification of heat transfer, mass transfer and residence time distribution and scale-up. Detailed scale-up methodology is presented with effect of relevant parameters for successful scale-up. Modular pilot plant with inline quenching, extraction and separation are some of the salient features presented in this work.10acontinuous flow10anitration10aPinched tube10aRTD10ascale-up1 aHussain, Arshad1 aSharma, Mrityunjay1 aPatil, Suneha1 aAcharya, Roopashree, B.1 aKute, Mahesh1 aWaghchaure, Aishwarya1 aKulkarni, Amol, A. uhttps://library.ncl.res.in/content/design-and-scale-continuous-di-nitration-reaction-using-pinched-tube-flow-reactor01605nas a2200241 4500008004100000022001400041245010400055210006900159260000900228300001600237490000700253520076200260653002001022653003201042653001601074653002401090653002701114100002201141700002601163700002401189700002301213856012701236 2021 eng d a0947-653900aMulti-step synthesis of miltefosine: integration of flow chemistry with continuous mechanochemistry0 aMultistep synthesis of miltefosine integration of flow chemistry cDEC  a17695-176990 v273 aHerein we report for the first time, an advanced continuous flow synthesis of the blockbuster Leishmaniasis drug miltefosine from simple starting materials by a sequence involving four steps of chemical transformation including a continuous mechanochemical step. First three reaction steps were performed in simple tubular reactors in a telescopic mode, while in the last step the product precipitated from the 3(rd) step was used for a continuous mechanochemical synthesis of miltefosine. When compared to a typical batch protocol that takes 15 h, miltefosine was obtained in 58 % overall yield in flow synthesis mode at the laboratory scale in a total residence time 34 min at synthesis rate of 10 g/hr, which is sufficient to treat 4800 patients per day.10acontinuous flow10acontinuous mechanochemistry10amiltefosine10amultistep synthesis10areactive intermediates1 aPatil, Niteen, B.1 aAtapalkar, Ranjit, S.1 aChavan, Subhash, P.1 aKulkarni, Amol, A. uhttps://library.ncl.res.in/content/multi-step-synthesis-miltefosine-integration-flow-chemistry-continuous-mechanochemistry02050nas a2200217 4500008004100000022001400041245008700055210006900142260000800211300001200219490000700231520134100238653002701579653001301606653002001619653001701639653001501656100002601671700002301697856011201720 2024 eng d a2062-249X00aContinuous flow ozonolysis of cardanol for greener synthesis of bio-based monomers0 aContinuous flow ozonolysis of cardanol for greener synthesis of  cJUN a417-4260 v143 a

Synthesis of bio-based monomers via continuous flow ozonolysis of cardanol using a simple tubular reactor is demonstrated. The direct ozonolysis of cardanol produces unique monomer 8-(3-hydroxyphenyl) octanal (HPOA) and heptanal along with several other oxidation products. Maximum 47% yield of HPOA with 54.3% conversion of cardanol was obtained at 0 degrees C in 9 s. The complete conversion of cardanol was obtained at the ozone to cardanol molar flow ratios greater than 2 at all temperatures varied in the range of -10 degrees C to 20 degrees C. Owing to large gas-liquid ratios, the mass transfer limitation for transfer of ozone from gas to liquid was negligible; however, the extent of axial dispersion in the liquid phase was significant at lower liquid flow rates. The non-ideal behavior was incorporated in the axial dispersion model to predict the conversion of cardanol. Examination of kinetic rates by both ideal plug-flow model and plug-flow with axial dispersion model revealed that the reaction is fast and is least influenced by the axial-dispersion in the reactor at prevailing operating conditions. The findings of the current study show that continuous flow technique enables a simple and safer synthesis of high-value bio-based monomers via ozonolysis of cardanol compared to traditional batch methods.

10aAxial-dispersion model10aCardanol10acontinuous flow10aHelical coil10aOzonolysis1 aKulkarni, Sphurti, P.1 aKulkarni, Amol, A. uhttps://library.ncl.res.in/content/continuous-flow-ozonolysis-cardanol-greener-synthesis-bio-based-monomers02014nas a2200241 4500008004100000245006700041210006700108260000800175300001100183490000700194520127900201653001501480653001901495653002001514653001701534653002001551653001301571100001901584700002401603700002001627700002601647856009901673 2024 eng d00aContinuous flow synthesis of hierarchical low silica X zeolite0 aContinuous flow synthesis of hierarchical low silica X zeolite cJUN a1090470 v393 a

Zeolites, renowned for their versatile applications in catalysis, adsorption, and ion exchange, have long been synthesized using conventional batch processes. However, the inherent limitations of these methods, such as resource-intensive conditions and inconsistent product quality, underscore the need for a sustainable and efficient approach. In this study, a continuous flow synthesis process was established for the synthesis of industrially important low silica X (LSX) zeolite using a tubular reactor. The synthesis gel was subjected to aging for 5 days at room temperature to facilitate nucleation and crystal growth combined with the fast-heating rate in a tubular reactor at 363 K & 1.1 atm., which in turn produces LSX after 40 min. The synthesized product was confirmed by the XRD, FE-SEM, EDS, XRF, TEM, and N2 adsorption-desorption; the data was compared with the LSX sample synthesized by batch process. The result implies that LSX prepared by continuous flow has a pure phase of LSX with the hierarchical structure, which provides better adsorption capacity of CO2 at 298 K up to 20 bar. Due to continuous flow synthesis, the crystallization time was reduced and faster kinetics which may be helpful for scale-up the process for LSX synthesis.

10aAdsorption10aCarbon dioxide10acontinuous flow10aLow silica X10aTubular reactor10azeolites1 aAdarsh, V., K.1 aShrotri, Aadesh, R.1 aBirje, Amit, R.1 aNandanwar, Sachin, U. uhttps://library.ncl.res.in/content/continuous-flow-synthesis-hierarchical-low-silica-x-zeolite02330nas a2200217 4500008004100000022001400041245020900055210007000264260000800334490000700342520144700349653002001796653002401816653002601840653002501866653002601891100001801917700001801935700002801953856013101981 2025 eng d a2193-580700aContinuous flow β-zeolite catalysed regioselective alkylation of naphthols using alcohols for synthesis of peroxynaphthalen-2(1H)-one, Azidonaphthalen-2(1H)-one and Fluoronaphthalen-2(1H)-one derivatives0 aContinuous flow βzeolite catalysed regioselective alkylation of  cAPR0 v143 a

Functionalized naphthols are prominent scaffolds in organic synthesis and materials chemistry. Herein, we demonstrated continuous flow alkylation of alpha- and beta-naphthols by using various primary and secondary benzylic alcohols in the presence of environmentally benign granular beta-zeolite as a reusable catalyst. For a variety of beta-naphthols, the respective alkylated products with good regioselectivity were obtained in high yields under mild reaction conditions. This protocol proceeded via the classical Friedel-Crafts type alkylation process and generated stable carbocations as intermediates. Applying this protocol, versatile naphthol derivatives have been synthesized using primary and secondary benzylic alcohols (50 and 44 examples in batch and continuous flow process, respectively), with good yields. Key advantages of this process includes rapid and efficient transformation, facilitates gram-scale synthesis, and generates water as the sole by-product. The most significant advantage is the continuous reusability of granular beta-zeolite, which further emphasizes the sustainability of the method. The application of alkylated naphthols for quaternary functionalization was demonstrated through peroxidation, azidation, and halogenation reactions under the continuous flow module, which yielded the respective peroxynaphthalen-2(1H)-one, azidonaphthalen-2(1H)-one and fluoronaphthalen2(1H)-one derivatives.

10acontinuous flow10aMultigram Synthesis10aReusable beta-zeolite10aSustainable Appraoch10aTransition metal free1 aLondhe, Gokul1 aBokade, Vijay1 aGnanaprakasam, Boopathy uhttps://library.ncl.res.in/content/continuous-flow-%CE%B2-zeolite-catalysed-regioselective-alkylation-naphthols-using-alcohols