HRID621751

反应详情

EQUATION

反应方程式

HRID 621751 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5.8 mmol of (3R,7R)-3,7,11-trimethyldodecyl bromide are heated at reflux for 1/4 hour in 20 ml of ethyl acetate with activated magnesium. Then, there are added at 0° C. 1 g of (S)-4-(2',5'-dimethoxy-3',4',6'-trimethylphenyl)-2-methyl-1,2-epoxybutane and 0.9 g of copper(I)-2-propylacetylide (or 1.2 g of copper(I) bromide/dimethyl sulphide complex). The temperature of the reaction mixture is subsequently left to rise to room temperature and the mixture is stirred overnight. 10 ml of ammonium with ethyl ether. The extract is dried and concentrated, and the residue is distilled in a bulb-tube (b.p.0.01 =140° C.). There are obtained 1.28 g (72%) (or 1.41 g (79%) of (3R,7R,11R)-1-)2',5'-dimethoxy-3',4',6'-trimethylphenyl)-3,7,11,15-tetramethylhexadecan-3-ol as a colourless oil.

WORKUP

后处理

  1. additionThen, there are added at 0° C
  2. waitThe temperature of the reaction mixture is subsequently left
  3. customto rise to room temperature
  4. customThe extract is dried
  5. concentrationconcentrated
  6. distillationthe residue is distilled in a bulb-tube (b.p.0.01 =140° C.)