HRID1275866

反应详情

EQUATION

反应方程式

HRID 1275866 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A mixture of t-butylcyclopentadiene (15 g, 123 mmol), acetone (9.0 mL, 135.2 mmol), pyrrolidine (11.7 mL, 135.3 mmol) and methanol (100 mL) was stirred at 0° C., for 30 minutes, and then at room temperature overnight. The reaction mixture was quenched with acetic acid (7.38 g) and with water (100 mL) at 0° C. The mixture was extracted with Et2O (3×200 mL); the organic layers were combined, washed with a saturated solution of NaHCO3, dried over anhydrous magnesium sulphate, filtered and finally concentrated, thus yielding 2-butyl-6,6-dimethylfulvene in the form of a yellow liquid (18.24 g, 92% yield).

WORKUP

后处理

  1. customat room temperature
  2. customovernight
  3. customThe reaction mixture was quenched with acetic acid (7.38 g) and with water (100 mL) at 0° C
  4. extractionThe mixture was extracted with Et2O (3×200 mL)
  5. washwashed with a saturated solution of NaHCO3
  6. dry with materialdried over anhydrous magnesium sulphate
  7. filtrationfiltered
  8. concentrationfinally concentrated