2-bromo-2-methoxypropiophenone synthesis
- Product Name:2-bromo-2-methoxypropiophenone
- CAS Number:135333-25-4
- Molecular formula:C10H11BrO2
- Molecular Weight:243.1
5561-92-2
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Yield:135333-25-4 99%
Reaction Conditions:
with copper(ll) bromide in chloroform;ethyl acetate; for 3 h;Heating / reflux;
Steps:
29
Combine 2'-hydroxypropiophenone (4.55 mL, 33.3 mmol) with cesium carbonate (11 g, 33.7 mmol) and iodomethane (4.1 mL, 65.8 mmol) in acetone (100 mL) and stir in a sealed vessel at RT until the reaction is complete. Concentrate the mixture and partition residue between water and EtOAc. Dry the combined extracts over Na2SO4 and concentrate. Chromatograph the resulting residue over silica gel (EtOAc/hexanes) to allow for isolation of 1-(2-methoxy-phenyl)-propan-1-one (5.01 g, 93 %). MS (ES): (M+1) + 165. 1 M/Z. Dissolve 1- (2-METHOXY-PHENYL)-PROPAN-1-ONE (5.0 g, 30.5 mmol) in CHC13 (25 mL) and add this mixture to a warmed slurry of CuBr2 (13.6 g, 60.1 mmol) in EtOAc (75 mL). Heat the resulting mixture near reflux for approx. 3 h. Cool and filter the mixture and concentrate the resulting filtrate. Chromatograph the resulting residue over silica gel (CH2CL2) to allow for isolation of 2-BROMO-1- (2-METHOXY-PHENYL)-PROPAN-1-ONE (7.32 g, 99 %). MS (ES): (M+1) + 243. 0,245. 0 M/Z.
References:
WO2005/19184,2005,A1 Location in patent:Page/Page column 76
7452-01-9
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135-02-4
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