HRID1616689

反应详情

EQUATION

反应方程式

HRID 1616689 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

30 g (106 mmol) of 3-bromo-5,5,8,8-tetramethyl-5,6,7,8-tetrahydronaphth-1-ol are dissolved in 500 mL of anhydrous THF. The medium is cooled to −78° C. and 156 mL (265 mmol) of tert-butyllithium are then added dropwise. After 45 minutes at this temperature, 12.3 mL (159 mmol) of dimethylformamide are added. The mixture is warmed to room temperature and then treated with 1N hydrochloric acid solution and extracted with ethyl acetate. The residue obtained is then purified by chromatography (eluent: 9/1 heptane/ethyl acetate). A white solid is obtained (m=16.5 g; yield=67%; m.p.=144° C.).

WORKUP

后处理

  1. temperatureThe mixture is warmed to room temperature
  2. extractionextracted with ethyl acetate
  3. customThe residue obtained
  4. customis then purified by chromatography (eluent: 9/1 heptane/ethyl acetate)
  5. customA white solid is obtained (m=16.5 g; yield=67%; m.p.=144° C.)