反応 #454041

反応方程式

n-Butyllithium

3,4-(ethylenedioxy)thiophene

Tributylstannyl chloride

→

2-(tributylstannyl)-3,4-(ethylenedioxy)thiophene

収率 98.0%

溶媒

THF

反応条件

後処理

1. 1
   温度to warm to room temperature
2. 2
   ろ過At room temperature the mixture was filtered
3. 3
   その他dried

実験手順

n-Butyllithium (77 mL, 192.5 mmol, 2.5 M solution in hexane) was added dropwise at -78° C. to a solution of 3,4-(ethylenedioxy)thiophene (25 g, 175.9 mmol) in anhydrous THF (100 mL) under nitrogen. The solution was stirred for 1 h and warmed to -40° C. Tributylstannyl chloride (85.89 g, 263.9 mmol) was added and the entire solution was finally allowed to warm to room temperature. At room temperature the mixture was filtered using Celite and the solvent was stripped. The organo-tin compound was vacuum dried to give 2-(tributylstannyl)-3,4-(ethylenedioxy)thiophene, obtained as a dark yellow liquid, yield=98%. MS(EI) m/z (rel int): 375 [(M)+ --C4H8, 100%] and 319[(M)+ --C8H16, 18%].

出典