HRID1174943

反应详情

EQUATION

反应方程式

HRID 1174943 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Dissolve N,N′-dimethyl-N-(6-nitro-benzothiazol-2-yl)-ethane-1,2-diamine (0.255 g, 0.957 mmol) in CH2Cl2 (10 mL) and add pyridine (0.1 mL, 1.2 mmol). Add acetyl chloride (0.102 mL, 1.43 mmol) and shake the mixture overnight at room temperature. Concentrate the reaction mixture in vacuo (adsorbing onto silica gel) and subject the mixture to silica gel flash column chromatography (40 g column, eluting with 1-10% MeOH/CH2Cl2) to yield the desired product (0.295 g, 100%). mass spectrum (m/e): 309.2 (M+1).

WORKUP

后处理

  1. customthe mixture overnight
  2. customat room temperature
  3. concentrationConcentrate the reaction mixture in vacuo (adsorbing onto silica gel)
  4. washto silica gel flash column chromatography (40 g column, eluting with 1-10% MeOH/CH2Cl2)