反応 #55075

反応方程式

potassium carbonate

p-chlorobenzylmercaptan

methyl chloroacetate

potassium iodide

→

methyl p-chlorobenzylmercapto-acetate

収率 100.0%

溶媒

acetone

反応条件

後処理

1. 1
   その他The mixture thus obtained
2. 2
   温度heated
3. 3
   温度under reflux for 7 hours
4. 4
   温度It is cooled
5. 5
   ろ過the precipitate (K2CO3) is filtered off
6. 6
   その他the acetone is evaporated from the filtrate
7. 7
   洗浄The ether solution is washed with 4 N NaOH
8. 8
   乾燥The ether solution is then dried over MgSO4
9. 9
   その他the ether is evaporated

実験手順

Anhydrous acetone (100 ml), potassium carbonate (21 g), p-chlorobenzylmercaptan (19.5 ml), methyl chloroacetate (13.2 ml) and potassium iodide (0.1 g) are mixed in the cold. The mixture thus obtained is stirred and heated under reflux for 7 hours. It is cooled, the precipitate (K2CO3) is filtered off, the acetone is evaporated from the filtrate and the residue is taken up with ether. The ether solution is washed with 4 N NaOH and then with water until the wash waters have a neutral pH. The ether solution is then dried over MgSO4, the ether is evaporated and 34.5 g (100% yield) of methyl p-chlorobenzylmercapto-acetate are collected in the form of a chromatographically pure oil.

出典