반응 #1137992

반응 방정식

7-(2,2-dimethyl-propionyloxy)-3-methyl-4-phenyl-isothiazolo[4,5-c]pyridine-6-carboxylic acid butyl ester

N-bromosuccinimide

→

title compound

수율 85.7%

3-Bromomethyl-7-(2,2-dimethyl-propionyloxy)-4-phenyl-isothiazolo[4,5-c]pyridine-6-carboxylic acid butyl ester

수율 85.7%

용매

CCl4

반응 조건

후처리

1. 1
   온도The reaction mixture was refluxed for 18 h
2. 2
   여과was filtered
3. 3
   농축The filtrate was concentrated in vacuo
4. 4
   기타purified by flash chromatography on silica gel
5. 5
   세척Eluting with 0-20% EtOAc/CH2Cl2

실험 절차

To a solution of 7-(2,2-dimethyl-propionyloxy)-3-methyl-4-phenyl-isothiazolo[4,5-c]pyridine-6-carboxylic acid butyl ester (392 mg) in CCl4 (1.8 mL) was added N-bromosuccinimide (172 mg) and benzoyl peroxide (11.1 mg). The reaction mixture was refluxed for 18 h. After cooling to r.t. the mixture was filtered. The filtrate was concentrated in vacuo and purified by flash chromatography on silica gel. Eluting with 0-20% EtOAc/CH2Cl2 gave the title compound (398 mg) as a yellow oil: MS (m/z) 505.1 (M+1), 507.1 (M+1).

출처