HRID1912110

反应详情

EQUATION

反应方程式

HRID 1912110 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

3-(2,2-dimethylpropyl)-1-cyclobutenecarboxylic acid (10 g), tetrahydrofuran (100 mL) and 6 N hydrochloric acid (100 mL) were mixed. To the mixture was added zinc (30 g) at ice temperature. The mixture was stirred at 70° C. overnight. After an addition of 6 N hydrochloric acid and water the mixture was filtered. The filtrate was extracted with ethyl acetate (150 mL, 100 mL). The organic layer was washed with brine (100 mL), then dried over sodium sulfate. The sodium sulfate was filtered off and the filtrate was concentrated in vacuo to give the title compound (11.6 g) as a crude product.

WORKUP

后处理

  1. filtrationwas filtered
  2. extractionThe filtrate was extracted with ethyl acetate (150 mL, 100 mL)
  3. washThe organic layer was washed with brine (100 mL)
  4. dry with materialdried over sodium sulfate
  5. filtrationThe sodium sulfate was filtered off
  6. concentrationthe filtrate was concentrated in vacuo