HRID352860

反应详情

EQUATION

反应方程式

HRID 352860 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In anhydrous tetrahydrofuran (500 ml), 6-ethoxycarbonyl-4,5,6,7-tetrahydrothiazolo[5,4-c]pyridine (WO94/21599) (21.0 g) was dissolved, followed by the addition of a solution of lithium aluminum hydride in tetrahydrofuran (a 1.0M solution, 200 ml) under ice cooling. The resulting mixture was stirred at room temperature for 2 hours. Water (7 ml) was then added slowly to the reaction mixture. After the termination of the reaction, a 1N aqueous potassium hydroxide solution (7 ml) and anhydrous magnesium sulfate were successively added. After removal of the insoluble matter by filtration, the filtrate was concentrated under reduced pressure. The residue thus obtained was purified by distillation under reduced pressure (1.5 mmHg, boiling point: 82 to 85° C.), whereby the title compound (6.10 g, 40%) was obtained as a colorless oil.

WORKUP

后处理

  1. customAfter the termination of the reaction
  2. customAfter removal of the insoluble matter
  3. filtrationby filtration
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. customThe residue thus obtained
  6. distillationwas purified by distillation under reduced pressure (1.5 mmHg, boiling point: 82 to 85° C.), whereby the title compound (6.10 g, 40%)
  7. customwas obtained as a colorless oil