HRID394547

反应详情

EQUATION

反应方程式

HRID 394547 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Diisopropylethylamine(5.7 mL, 3.27 mmol, 5.0 eq) was added to a mixture of camphorsulfonate salt (9) (3.4 g, 6.53 mmol) in CH2Cl2 (21 mL, 0.3 M) and followed by dropwise addition of PhCOCl (0.83 mL, 7.19 mmol, 1.1 eq). The solution was stirred at room temperature for 1 hour. The reacting mixture was diluted with CH2Cl2 (200 mL) and washed with brine, 1 M KHSO4, and saturated NaHCO3 then dried over MgSO4. The concentrated crude oil was purified by flash chromatography (CH2Cl2-MeOH/95:5) to give white solid (2.30 g, 89.8%).

WORKUP

后处理

  1. washwashed with brine, 1 M KHSO4, and saturated NaHCO3
  2. dry with materialthen dried over MgSO4
  3. concentrationThe concentrated crude oil
  4. customwas purified by flash chromatography (CH2Cl2-MeOH/95:5)