HRID2307820

反应详情

EQUATION

反应方程式

HRID 2307820 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of t-butyl N-(2,3-dihydroxypropyl)carbamate (9.0 g, 47 mmol) in CH2Cl2 (75 mL) was added t-butyldimethylsilyl chloride (7.80 g, 51.7 mmol), triethylamine (7.86 mL, 56.4 mmol) and DMAP (230 mg). The solution was stirred at rt overnight. After diluting with CH2Cl2 (50 mL), the solution was washed with water (2×100 mL), dried over MgSO4 and concentrated. The residual oil was distilled by Kugelrohr under vacuum to give the desired product (13.6 g, 95%). MS (DCI) m/z 306 (M+1)+.

WORKUP

后处理

  1. washthe solution was washed with water (2×100 mL)
  2. dry with materialdried over MgSO4
  3. concentrationconcentrated
  4. distillationThe residual oil was distilled by Kugelrohr under vacuum