反応 #1185936

反応方程式

product

1-(3-Chloro-4-mercapto-phenyl)ethanone

sodium hydride

4-iodo-tetrahydro-pyran

→

desired product

収率 32.0%

1-[3-Chloro-4-(tetrahydro-pyran-4-ylsulfanyl)-phenyl]-ethanone

収率 32.0%

溶媒

DMF

反応条件

後処理

1. 1
   その他The reaction mixture was quenched with water at 0° C. and neutralized with trifluoroacetic acid
2. 2
   その他Evaporation and purification of the crude product by silica gel chromatography

実験手順

The product from step 1 (3.0 g, 16.07 mmol) was added to a suspension of sodium hydride (964.3 mg, 32.14 mmol) in DMF at 0° C. After 5 min 4-iodo-tetrahydro-pyran (3.41 g, 16.07 mmol) was added and the reaction mixture was stirred at RT for 1 h. The reaction mixture was quenched with water at 0° C. and neutralized with trifluoroacetic acid. Evaporation and purification of the crude product by silica gel chromatography using ethyl acetate/n-heptane gave the desired product (1.385 g, 32%)

出典