HRID384239

反应详情

EQUATION

反应方程式

HRID 384239 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a cooled (−70° C.) mixture of thiophene (17.6 g, 0.21 mol) in anhydrous THF (100 mL) was added dropwise a solution of n-BuLi (137.5 ml, 1.6 M, 0.22 mol) in hexane. After stirring for 1 hour at 0° C., the mixture was cooled to −40° C. followed by addition of 1-hexylbromide (0.22 mol). The mixture was slowly heated to r.t. Water (250 mL) was added and the mixture was extracted with diethylether (3×150 mL). The combined organic fractions were dried over MgSO4 and concentrated in vacuo. The product was purified by means of vacuum distillation. This product was prepared according to the general procedure and obtained as a colourless oil (26.5 g, 75%).

WORKUP

后处理

  1. temperatureTo a cooled
  2. temperaturethe mixture was cooled to −40° C.
  3. temperatureThe mixture was slowly heated to r.t
  4. extractionthe mixture was extracted with diethylether (3×150 mL)
  5. dry with materialThe combined organic fractions were dried over MgSO4
  6. concentrationconcentrated in vacuo
  7. distillationThe product was purified by means of vacuum distillation
  8. customThis product was prepared