HRID390702

反应详情

EQUATION

反应方程式

HRID 390702 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 5-methylthiazol-2-amine (4.8 g, 42 mmol), N,N-carbonyldiimidazole (9.8 g, 61 mmol), and 4-dimethylaminopyridine (0.1 g, 1.0 mmol) in tetrahydrofuran (90 mL) was heated at 65° C. for 6 hours. Pyrrolidine (5.1 mL, 61 mmol) was then added and heating was continued at 65° C. for 48 hours. The mixture was concentrated, and the residue was diluted with methanol and then triturated with diethyl ether. The solids were collected by filtration, washed with diethyl ether, and recrystallized from ethyl acetate to give the title compound.

WORKUP

后处理

  1. temperatureheating
  2. concentrationThe mixture was concentrated
  3. additionthe residue was diluted with methanol
  4. customtriturated with diethyl ether
  5. filtrationThe solids were collected by filtration
  6. washwashed with diethyl ether
  7. customrecrystallized from ethyl acetate