2-BROMO-1-(5-METHYL-THIOPHEN-2-YL)-ETHANONE synthesis
- Product Name:2-BROMO-1-(5-METHYL-THIOPHEN-2-YL)-ETHANONE
- CAS Number:10531-42-7
- Molecular formula:C7H7BrOS
- Molecular Weight:219.0989
Yield:10531-42-7 1.7 g
Reaction Conditions:
Stage #1: 2-Bromoacetyl bromidewith triethylamine in dichloromethane; for 0.333333 h;
Stage #2: 2-Methylthiophene in dichloromethane;
Steps:
1b Example 1b
Example 1b A solution of Bromoacetylbromide (1.6 ml, 18.8 mmol) dissolved in 10 ml of DCM is added dropwise to a stirred solution of triethylamine (5.2 ml, 37.6 mmol) dissolved in 50 ml of DCM. After 20 minutes stirring, a solution of 2-Methylthiophene (1.2 g, 12.5 mmol) is added and the reaction mixture is stirred overnight. 50 ml of icy water are added and after 30 minutes stirring the mixture is extracted with DCM. The organic layer is separated, washed with brine, dried and concentrated under reduced pressure. The residue is purified by silica gel flash chromatography, using cyclohexane/EtOAc 95:5 to 70:30 as eluent, to obtain 1.7 g of the title compound. [0225] UPLC-MS (Method 1): Rt=1.07 min [0226] MS (ES+): m/z=219-221 [M+H]+
References:
US2015/105397,2015,A1 Location in patent:Paragraph 0223; 0224; 0225; 0226
