HRID493461

反应详情

EQUATION

反应方程式

HRID 493461 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

To a cooled (0° C.) solution of MeLi (13.0 mL; 21 mmol; 1.6 M in Et2O) was added 2-(trimethylsilyloxy)propene (2.8 g; 21 mmol). The solution was stirred 30 minutes at 0° C., and then warmed to room temperature and was stirred for 1 hour. The mixture was recooled to 0° C., and (4R,5R)-2-allyl-2-chloro-4,5-bis-(1-methoxy-1-methyl-ethyl)-[1,3,2]dioxasilolane (6.6 g; 21 mmol) was added. The mixture was warmed to room temperature and stirred for 2 hours. The solution was diluted with pentane (20 mL), and the mixture was then filtered through a pad of celite. The filtrate was concentrated, and the residue was distilled under reduced pressure to give 3.0 g (43%) of (4R,5R)-2-allyl-2-isopropenyloxy-4,5-bis-(1-methoxy-1-methyl-ethyl)-[1,3,2]dioxasilolane as a clear, colorless liquid.

WORKUP

后处理

  1. temperaturewarmed to room temperature
  2. stirringwas stirred for 1 hour
  3. customwas recooled to 0° C.
  4. temperatureThe mixture was warmed to room temperature
  5. stirringstirred for 2 hours
  6. filtrationthe mixture was then filtered through a pad of celite
  7. concentrationThe filtrate was concentrated
  8. distillationthe residue was distilled under reduced pressure