反応 #217553

反応方程式

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

ethyl 2-mercaptoacetate

triethylamine

→

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

溶媒

CH2Cl2

反応条件

後処理

1. 1
   その他to come to room temperature
2. 2
   その他(12 h)
3. 3
   ろ過The resulting suspension was filtered
4. 4
   洗浄the filtrate washed with water (100 ml) and brine (100 ml)
5. 5
   乾燥dried over Na2SO4
6. 6
   その他Removal of the solvent in vacuo
7. 7
   その他gave a slightly yellow oil, which
8. 8
   その他was purified by flash chromatography (ethyl acetate-petroleum ether 1:25)

実験手順

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).

出典