HRID1789604

反应详情

EQUATION

反应方程式

HRID 1789604 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

5.8 mmol of (3R,7R)-3,7,11-trimethyl-dodecyl bromide are heated at reflux for 1/4 hour in 20 ml of diethyl ether with etched magnesium. 1 g of (S)-4-(2',5'-dimethoxy-3',4',6'-trimethylphenyl)-2-methyl-1,2-epoxy-butane and 0.9 g of copper(I) 2-propylacetylide (or 1.2 g of copper(I) bromide-dimethyl sulphide complex) are then added at 0° C. The temperature of the reaction mixture is subsequently left to rise to room temperature and the mixture is stirred for about 16 hours. 10 ml of ammonium chloride are then added and the mixture is extracted with diethyl ether. The extract is dried, concentrated and 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-tetramethyl-hexadecan-3-ol as a colourless oil, [α]D20 -0.67° (c=0.9% in CHCl3).

WORKUP

后处理

  1. waitThe temperature of the reaction mixture is subsequently left
  2. customto rise to room temperature
  3. extractionthe mixture is extracted with diethyl ether
  4. customThe extract is dried
  5. concentrationconcentrated
  6. distillationdistilled in a bulb-tube (b.p.0.01 =140° C.)