HRID1169569

反应详情

EQUATION

反应方程式

HRID 1169569 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

1-Bromo-3-ethoxypropane (5.85 g, 35.0 mmol) was dissolved in THF (30 mL). Magnesium (900 mg, 37.0 mmol) and iodine (catalytic amount) were added thereto, and the resultant mixture was stirred at room temperature for 30 minutes and at 60° C. for 10 minutes. The resultant mixture was added dropwise to diisopropylchlorosilane (5.12 mL, 30.0 mmol) in THF (40 mL), followed by stirring at room temperature for 15 minutes and at 60° C. for 1.5 hours. Saturated aqueous ammonium chloride was added thereto, and the resultant mixture was extracted with pentane, followed by washing with water six times and drying over sodium sulfate anhydrate. The solvent was removed under reduced pressure, whereby the Compound 61a was obtained as an yellow liquid (6.52 g, 92%).

WORKUP

后处理

  1. extractionthe resultant mixture was extracted with pentane
  2. washby washing with water six times
  3. dry with materialdrying over sodium sulfate anhydrate
  4. customThe solvent was removed under reduced pressure, whereby the Compound 61a