HRID531105

反应详情

EQUATION

反应方程式

HRID 531105 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2M aqueous sodium hydroxide solution (20 mL) was added to a solution of methyl 6-(1-((6-cyclopropyl-2,4′-difluoro-3-isopropoxybiphenyl-4-yl)methyl)piperidin-4-yl)-2-ethyl-5-oxo-5,6,7,8-tetrahydro-1,6-naphthyridine-3-carboxylate (8.03 g) in methanol (25 mL) at 70° C. The mixture was stirred at the same temperature under nitrogen atmosphere for 2 hours. The mixture was neutralized with 1M hydrochloric acid at room temperature and added to water (100 mL). The mixture was stirred at 70° C. for 30 minutes and at room temperature for 2 hours to give colorless crystals. After filtration, the crystals were dissolved in ethanol. The solution was filtrated and the filtrate was concentrated in vacuo to give a colorless solid. The solid was recrystallized from ethanol-water (45 mL-130 mL) to give the title compound (7.26 g).

WORKUP

后处理

  1. stirringThe mixture was stirred at 70° C. for 30 minutes and at room temperature for 2 hours
  2. customto give colorless crystals
  3. filtrationAfter filtration
  4. dissolutionthe crystals were dissolved in ethanol
  5. filtrationThe solution was filtrated
  6. concentrationthe filtrate was concentrated in vacuo
  7. customto give a colorless solid
  8. customThe solid was recrystallized from ethanol-water (45 mL-130 mL)