In Situ Investigation of Multicomponent MOF Crystallization during Rapid Continuous Flow Synthesis

Herein the anti-influenza drug (–)-oseltamivir phosphate is prepared in continuous flow from ethyl shikimate with 54% overall yield over nine steps and total residence time of 3.5 min from the individual steps. Although the procedure involved intermediate isolation, the dangerous azide chemistry and intermediates involved were elegantly handled in situ. It is the first continuous-flow process for (–)-oseltamivir phosphate involving azide chemistry and (–)-shikimic acid as precursor.

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One-Step Continuous Flow Synthesis of Highly Substituted Pyrrole-3-carboxylic Acid Derivatives via in Situ Hydrolysis oftert-Butyl Esters

Organic Letters ◽

10.1021/ol102216x ◽

2010 ◽

Vol 12 (22) ◽

pp. 5182-5185 ◽

Cited By ~ 58

Author(s):

Ananda Herath ◽

Nicholas D. P. Cosford

Keyword(s):

Carboxylic Acid ◽

Continuous Flow ◽

Flow Synthesis ◽

Butyl Esters ◽

One Step

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The in situ generation and reactive quench of diazonium compounds in the synthesis of azo compounds in microreactors

Beilstein Journal of Organic Chemistry ◽

10.3762/bjoc.12.186 ◽

2016 ◽

Vol 12 ◽

pp. 1987-2004 ◽

Cited By ~ 8

Author(s):

Faith M Akwi ◽

Paul Watts

Keyword(s):

Continuous Flow ◽

Coupling Reaction ◽

Azo Compounds ◽

Coupling Reactions ◽

Azo Coupling ◽

Reaction Conditions ◽

Flow Rates ◽

Flow Synthesis ◽

Optimum Flow

In this paper, a micro-fluidic optimized process for the continuous flow synthesis of azo compounds is presented. The continuous flow synthesis of Sudan II azo dye was used as a model reaction for the study. At found optimal azo coupling reaction temperature and pH an investigation of the optimum flow rates of the reactants for the diazotization and azo coupling reactions in Little Things Factory-MS microreactors was performed. A conversion of 98% was achieved in approximately 2.4 minutes and a small library of azo compounds was thus generated under these reaction conditions from couplers with aminated or hydroxylated aromatic systems. The scaled up synthesis of these compounds in PTFE tubing (i.d. 1.5 mm) was also investigated, where good reaction conversions ranging between 66–91% were attained.

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In situ investigation of the primary recrystallization of alpha titanium in HVEM

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100110313 ◽

1978 ◽

Vol 36 (1) ◽

pp. 634-635

Author(s):

S. Naka ◽

R. Penelle ◽

R. Valle

Keyword(s):

Dimensional Analysis ◽

Texture Evolution ◽

Cold Work ◽

Three Dimensional ◽

Primary Recrystallization ◽

Thin Foils ◽

In Situ Investigation ◽

Grain Growth Model ◽

Alpha Titanium

The in situ experimentation technique in HVEM seems to be particularly suitable to clarify the processes involved in recrystallization. The material under investigation was unidirectionally cold-rolled titanium of commercial purity. The problem was approached in two different ways. The three-dimensional analysis of textures was used to describe the texture evolution during the primary recrystallization. Observations of bulk-annealed specimens or thin foils annealed in the microscope were also made in order to provide information concerning the mechanisms involved in the formation of new grains. In contrast to the already published work on titanium, this investigation takes into consideration different values of the cold-work ratio, the temperature and the annealing time.Two different models are commonly used to explain the recrystallization textures i.e. the selective grain growth model (Beck) or the oriented nucleation model (Burgers). The three-dimensional analysis of both the rolling and recrystallization textures was performed to identify the mechanismsl involved in the recrystallization of titanium.

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