HRID1862748

反应详情

EQUATION

反应方程式

HRID 1862748 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a cold (−78° C.) solution of 2,2-dimethyl-4(2-methyl-thien-5-yl)-6-bromo-thiochrom-3-ene (Compound T, 430 mg, 1.2 mmol) in THF (12 mL) was added n-BuLi in hexane (1.6 M solution, 1 mL). The mixture was gradually warmed to ambient temperature over 1 hour and recooled to −78° C. To this solution was added DMF (220 mg, 3 mmol) and the mixture was stirred at ambient temperature for 16 hours. The reaction was quenched by adding water (10 mL) and ethy lacetate (100 mL). The organic layer was washed with brine (10 mL), dried and the solvent was removed by distillation to obtain the title compound as a pale yellow oil.

WORKUP

后处理

  1. customrecooled to −78° C
  2. customThe reaction was quenched
  3. additionby adding water (10 mL) and ethy lacetate (100 mL)
  4. washThe organic layer was washed with brine (10 mL)
  5. customdried
  6. customthe solvent was removed by distillation