反応 #77310

反応方程式

1-(2-hydroxyethyl)-4-(2-fluorophenyl)piperazine

pyridine

Thionyl chloride

→

desired product

収率 18.0%

1-(2-Chloroethyl)-4-(2-fluorophenyl)piperazine

収率 18.0%

溶媒

benzene

反応条件

後処理

1. 1
   その他was immersed in a 60° C.
2. 2
   その他for 1 hour
3. 3
   その他The layers were separated
4. 4
   抽出the aqueous fraction was extracted with ethyl acetate (2×20 mL)
5. 5
   乾燥The combined organic fractions were dried over sodium sulfate
6. 6
   その他the solvent was removed in vacuo

実験手順

Thionyl chloride (1 mL) was added dropwise to an ice-cooled solution of 1-(2-hydroxyethyl)-4-(2-fluorophenyl)piperazine (300 mg) and pyridine (1 mL) in benzene (20 mL). After 30 minutes the solution was brought to room temperature and then the flask was immersed in a 60° C. oil bath for 1 hour. The layers were separated and the aqueous fraction was extracted with ethyl acetate (2×20 mL). The combined organic fractions were dried over sodium sulfate and the solvent was removed in vacuo, giving the desired product as a yellow solid (58.6 mg, 18%). ESI-MS m/z 243 (MH+).

出典