HRID1361910

反应详情

EQUATION

反应方程式

HRID 1361910 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
5 °C

PROCEDURE

实验过程

In a 1-L 4-necked round-bottom flask, 3,3-dimethylhex-5-enal (14.20 g; 0.113 mol) was dissolved in absolute ethanol (420 mL). Then the mixture was cooled to 5° C. in an ice-bath and, under nitrogen atmosphere, sodium borohydride (3.3 g; 0.087 mol) was added cautiously in 10 minutes. After the mixture had been stirred for 1 hour, it was poured into 5% ammonium chloride, diluted with water, and extracted with dichloromethane. Extracts were dried over sodium sulfate and evaporated, then the white solid was filtered away, while the pale yellow oil was distilled at 55-56° C. (4 mmHg) to give the title compound as a foul smelling, colorless liquid.

WORKUP

后处理

  1. extractionextracted with dichloromethane
  2. dry with materialExtracts were dried over sodium sulfate
  3. customevaporated
  4. filtrationthe white solid was filtered away, while the pale yellow oil
  5. distillationwas distilled at 55-56° C. (4 mmHg)