反応 #3759

反応方程式

2,5-dichlorophenylthioacetic acid

thionyl chloride

→

2,5-dichlorophenyl-thioacetyl chloride

収率 106.5%

溶媒

methylene chloride

反応条件

後処理

1. 1
   温度at reflux for 3 h
2. 2
   濃縮was concentrated in vacuo
3. 3
   その他The residue was evaporated two times from toluene

実験手順

A solution of 2,5-dichlorophenylthioacetic acid (13.0 g, 54.9 mmol) in methylene chloride (55 mL) and thionyl chloride (10 mL, 137 mmol) was heated at reflux for 3 h. The reaction mixture was allowed to cool to room temperature and was concentrated in vacuo. The residue was evaporated two times from toluene to give 14 g of 2,5-dichlorophenyl-thioacetyl chloride (100% yield) as a slightly colored product which was used in the next step without purification. 1H NMR (300 MHz, CDCl3) δ4.13 (s, 2H), 7.22 (dd, J=2, 9 Hz, 1H), 7.35 (d, J=9 Hz, 1H), 7.39 (d, J=2 Hz, 1H).

出典