HRID2085531

反应详情

EQUATION

反应方程式

HRID 2085531 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of gave N1-(2-chloro-5,6-dimethyl-3-nitropyridin-4-yl)-2-methylpropane-1,2-diamine (3.14 g, 10.9 mmol) in 50 mL of CH2Cl2 was cooled to 0° C. under N2 and treated with triethylamine (2.84 mL, 20.4 mmol) and acetic anhydride (1.01 mL, 10.7 mmol). After stirring for 2 h, the reaction was quenched by the addition of saturated aqueous NaHCO3. CH2Cl2 (100 mL) was added and the organic layer was separated. The organic layer was then washed with cold H2O (2×) and brine. The organic portion was dried with Na2SO4 and concentrated to give N-{2-[(2-chloro-5,6-dimethyl-3-nitropyridin-4-yl)amino]-1,1-dimethylethyl}acetamide (2.80 g) as a yellow foam.

WORKUP

后处理

  1. customthe reaction was quenched by the addition of saturated aqueous NaHCO3
  2. additionCH2Cl2 (100 mL) was added
  3. customthe organic layer was separated
  4. washThe organic layer was then washed with cold H2O (2×) and brine
  5. dry with materialThe organic portion was dried with Na2SO4
  6. concentrationconcentrated