반응 #217553

반응 방정식

2-bromo-2-methyl-pentan-3-one

ethyl 2-mercaptoacetate

triethylamine

→

ethyl[(1,1-dimethyl-2-oxobutyl)thio]acetate

용매

CH2Cl2

반응 조건

후처리

1. 1
   기타to come to room temperature
2. 2
   기타(12 h)
3. 3
   여과The resulting suspension was filtered
4. 4
   세척the filtrate washed with water (100 ml) and brine (100 ml)
5. 5
   건조dried over Na2SO4
6. 6
   기타Removal of the solvent in vacuo
7. 7
   기타gave a slightly yellow oil, which
8. 8
   기타was purified by flash chromatography (ethyl acetate-petroleum ether 1:25)

실험 절차

To a solution of 2-bromo-2-methyl-pentan-3-one (A1) (13.5 g, 75 mmol) in CH2Cl2 (400 ml) were added ethyl 2-mercaptoacetate (9 g, 8.2 ml, 75 mmol) and 10.42 ml triethylamine at 0° C. and stirred for 3 h. The solution was allowed to come to room temperature (12 h). The resulting suspension was filtered, the filtrate washed with water (100 ml) and brine (100 ml) and dried over Na2SO4. Removal of the solvent in vacuo gave a slightly yellow oil, which was purified by flash chromatography (ethyl acetate-petroleum ether 1:25).

출처