3-Bromopropionic acid synthesis
- Product Name:3-Bromopropionic acid
- CAS Number:590-92-1
- Molecular formula:C3H5BrO2
- Molecular Weight:152.97
598-72-1
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590-92-1
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Yield:590-92-1 79%
Reaction Conditions:
with tetrabutyl phosphonium bromide at 160; under 760.051 Torr; for 20 h;
Steps:
61 EXAMPLE 61 - 3-BrPA synthesis from 2-BrPA with [PBu4IBr molten salt catalyst
46.23 g of solid tetrabutylphosphonium bromide ([PBu4IBr; 133.5 mmol, 98%; Sigma-Aldrich Chemie GmbH, Taufkirchen, Germany; catalog 189138) were mixed with 20.68g of liquid 2-bromopropionic acid (2-BrPA; 133.5 mmol, 99%; Sigma-Aldrich Chemie GmbH, Taufkirchen, Germany; catalog B78300) in a 100 mL three-necked glass reactor in a molar ratio of 1:1 at room temperature and atmospheric conditions. The isomerization mixture was heated to 160°C under continuous stirring with a magnetic stirring bar at a speed of 450 rpm. Theisomerization mixture was batchwise refluxed and gaseous by-products were routed to the off-gas or collected in a hydrostatic colunm. After an overall process time of 20 h, the hot reaction mixture was allowed to cool down to room temperature and was analyzed via off-line ‘H NMR (JEOL ECX 400 MHz). ‘H qNMR analysis of the isomerization mixture gave a 3-bromopropionic acid (3- BrPA) yield of about 79 mol% and selectivity of more than about 90 mol%.
References:
THE PROCTER & GAMBLE COMPANY;ALBERT, Jakob;WASSERSCHEID, Peter;TACCARDI, Nicola;NAGENGAST, Jens;KEHRER, Matthias;KADAR, Julian;COLLIAS, Dimitris, Ioannis WO2018/22826, 2018, A1 Location in patent:Page/Page column 67
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590-92-1
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590-92-1
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107-94-8
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598-72-1
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598-78-7
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109-78-4
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590-92-1
238 suppliers
$10.00/1g