HRID323028

反应详情

EQUATION

反应方程式

HRID 323028 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

To a solution of 3-methoxythiophene (4.81 g, 42.1 mmol) in ether (20 mL) at −78° C., butyllithium (17 mL, 47.6 mmol) was added. The reaction mixture was stirred at −78° C. for 1 hour, then it was warmed to 0° C. for 3 hours. After to recooling −78° C. the reaction mixture was poured into a beaker filled with crushed dry ice (14.5 g) and allowed to stand until the excess dry ice had completely sublimed. Then the reaction mixture was poured into a mixture of ice (10 g) to which conc. HCl (24 mL) had been added. The product was purified by precipitation from ether and filtering (6.42 g, 96%). EI-MS m/z 159 (M+H)+.

WORKUP

后处理

  1. temperatureit was warmed to 0° C. for 3 hours
  2. additionAfter to recooling −78° C. the reaction mixture was poured into a beaker
  3. additionhad been added
  4. customThe product was purified by precipitation from ether
  5. filtrationfiltering (6.42 g, 96%)