HRID1398231

反应详情

EQUATION

反应方程式

HRID 1398231 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 2-{(8R)-3-[6-methoxy-5-(4-methyl-1H-imidazol-1-yl)pyridin-2-yl]-8-(3,4,5-trifluorophenoxy)-5,6,7,8-tetrahydro[1,2,4]triazolo[4,3-a]pyridin-8-yl}propan-2-ol (1.0 g) in 2-propanol (4 mL) was added a mixture of phosphoric acid (0.27 g) in 2-propanol (2 mL) at 50° C., and the mixture was stirred for 30 min. To the reaction mixture was added IPE (6 mL) at 50° C., and the mixture was stirred for 30 min. To the reaction mixture was added IPE (2 mL) at room temperature, and the mixture was stirred for 30 min. The crystals were collected by filtration, washed with IPE (2 mL) and dried to give the title compound (1.08 g).

WORKUP

后处理

  1. additionwas added
  2. additionTo the reaction mixture was added IPE (6 mL) at 50° C.
  3. stirringthe mixture was stirred for 30 min
  4. additionTo the reaction mixture was added IPE (2 mL) at room temperature
  5. stirringthe mixture was stirred for 30 min
  6. filtrationThe crystals were collected by filtration
  7. washwashed with IPE (2 mL)
  8. customdried