HRID1893408

反应详情

EQUATION

反应方程式

HRID 1893408 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a suspension of 2-piperazinone (5.3 g, 52.9 mmol) in dry dichloromethane (DCM) (76 ml) was added triethylamine (16.23 ml, 116 mmol) and finally 2,3-dichlorobenzoyl chloride (12.20 g, 58.2 mmol) dropwise (exothermic). The mixture was stirred at room temperature. After 1 hour the mixture was diluted with DCM (150 mL) and sat. NaHCO3 (150 ml), the phases were separated and the aqueous layer extracted with DCM (2×100 ml). The combined organic fractions were washed with brine and dried over MgSO4. Evaporation gave 4-[(2,3-dichlorophenyl)carbonyl]-2-piperazinone (12 g).

WORKUP

后处理

  1. customthe phases were separated
  2. extractionthe aqueous layer extracted with DCM (2×100 ml)
  3. washThe combined organic fractions were washed with brine
  4. dry with materialdried over MgSO4
  5. customEvaporation