HRID36908

反应详情

EQUATION

反应方程式

HRID 36908 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.6 g (0.005 mole) of 2-(5-methylthien-2-yl)imidazo[2,1-b]-benzothiazole-3-acetic acid are treated, at room temperature, with 0.85 g (0.005 mole) of N,N'-carbonyldiimidazole in 30 ml of anhydrous tetrahydrofuran for 3 h 30 min. The mixture is cooled using an ice bath, an excess of ammonia in 10 ml of anhydrous tetrahydrofuran cooled to -10° C. is added, and the mixture is stirred for 4 h at room temperature. The solvent is evaporated under reduced pressure, the solid is collected by filtration, it is washed with water up to neutral pH, then with ethanol, and finally with ethyl ether. After recrystallization from methanol, 1 g of a beige compound is obtained. Melting point: 243°-245° C.

WORKUP

后处理

  1. temperatureThe mixture is cooled
  2. additionis added
  3. customThe solvent is evaporated under reduced pressure
  4. filtrationthe solid is collected by filtration, it
  5. washis washed with water up to neutral pH
  6. customAfter recrystallization from methanol