HRID233780

反应详情

EQUATION

反应方程式

HRID 233780 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 room temperature for 1 hr. The CH2Cl2 solution was extracted with water and 1N HCl. The organic solution was washed with a saturated NaHCO3 solution and with a 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 a saturated NaHCO3 solution and with a brine solution
  3. dry with materialThe CH2Cl2 solution was dried (MgSO4)
  4. concentrationconcentrated in vacuo