反応 #11764

反応方程式

4-chloro-2-chloromethyl-1-methoxybenzene

cesium carbonate

thioacetic acid

→

title compound

収率 96.0%

Thioacetic acid S-(5-chloro-2-methoxy-benzyl)ester

収率 96.0%

溶媒

ethyl acetate

dimethylformamide

反応条件

後処理

1. 1
   洗浄washed with water, 5% aqueous sodium hydrogen carbonate, and brine
2. 2
   その他The organic layer was separated
3. 3
   乾燥dried over sodium sulfate
4. 4
   ろ過filtered
5. 5
   濃縮concentrated in vacuo

実験手順

To a solution of cesium carbonate (0.55 g, 1.70 mmol) in dimethylformamide (13 mL) was added thioacetic acid (0.24 g, 3.14 mmol) followed by addition of 4-chloro-2-chloromethyl-1-methoxybenzene (0.50 g, 2.62 mmol) in one portion. The reaction was stirred in the dark at ambient temperature overnight. The reaction was diluted with ethyl acetate, washed with water, 5% aqueous sodium hydrogen carbonate, and brine. The organic layer was separated, dried over sodium sulfate, filtered and concentrated in vacuo. Chromatography on silica gel gave the title compound (0.58 g).

出典