HRID5427

反应详情

EQUATION

反应方程式

HRID 5427 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of (±)-6-acetyl-4-(di-n-propylamino)-1,2,2a,3,4,5-hexahydrobenz[cd]indole (2.3 g, 7.7 mmol) and triethylamine (1.1 ml, 8 mmol) in 90 ml CH2Cl2 under N2 was added dropwise a solution of 2,2,2-trichloroethyl chloroformate. The reaction mixture was stirred at RT for 1 hr. The CH2Cl2 solution was extracted with water and 1N HCl. The organic solution was washed with saturated NaHCO3 solution and with brine solution. The CH2Cl2 solution was dried (MgSO4) and concentrated in vacuo to give 3.3 g of the 1-carbamylindoline.

WORKUP

后处理

  1. extractionThe CH2Cl2 solution was extracted with water and 1N HCl
  2. washThe organic solution was washed with saturated NaHCO3 solution and with brine solution
  3. dry with materialThe CH2Cl2 solution was dried (MgSO4)
  4. concentrationconcentrated in vacuo