HRID1174942

反应详情

EQUATION

反应方程式

HRID 1174942 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Dissolve 2-chloro-6-nitro-benzothiazole (2.20 g, 10.3 mmol) in THF (50 mL). Add N,N′-dimethyl-ethane-1,2-diamine (10.0 mL) and stir overnight at room temperature. Concentrate the reaction mixture in vacuo (adsorbing onto silica gel). Subject the mixture to silica gel flash column chromatography (120 g column, eluting with 10% 2N NH3 in MeOH/CH2Cl2) to yield the desired product (0.500 g, 18%). mass spectrum (m/e): 267.3 (M+1).

WORKUP

后处理

  1. concentrationConcentrate the reaction mixture in vacuo (adsorbing onto silica gel)
  2. washto silica gel flash column chromatography (120 g column, eluting with 10% 2N NH3 in MeOH/CH2Cl2)