HRID1954997

反应详情

EQUATION

反应方程式

HRID 1954997 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Chloroethyl chloroformate (12.4 g, 81 mmol) dissolved in dichloromethane (40 ml) is added dropwise at RT, during the course of about 30 min, to a solution of 8-(2-amino-6-methylbenzylamino)-2,3-dimethylimidazo[1,2-a]pyridine (19.65 g, 70 mmol) in anhydrous dichloromethane (600 ml). The mixture is then stirred at RT for 16 h and then extracted with sodium hydrogen carbonate (4×200 ml). After extraction of the aqueous phases with dichloromethane (200 ml), the combined organic extracts are washed with water (2×200 ml), dried over magnesium sulfate and concentrated. The crude product which remains (33.9 g) is used directly for the further reaction in Example 1b.

WORKUP

后处理

  1. extractionextracted with sodium hydrogen carbonate (4×200 ml)
  2. extractionAfter extraction of the aqueous phases with dichloromethane (200 ml)
  3. washthe combined organic extracts are washed with water (2×200 ml)
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated
  6. customis used directly for the further reaction in Example 1b