HRID873523

反应详情

EQUATION

反应方程式

HRID 873523 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Sodium carbonate (122 mg, 1.15 mmol) was added to a suspension of the 6-[4-methoxy-3-(3,3,6,6-tetramethyl-1,8-dioxo-2,3,4,5,6,7,8,9-octahydro-1H-xanthen-9-yl)phenyl]pyridine-2-carbonitrile produced in Example 6 (410 mg, 0.85 mmol) and hydroxylamine hydrochloride (73.8 mg, 1.06 mmol) in methanol (8.2 ml) at room temperature, and the mixture thus obtained was then stirred at the same temperature as above for 25 hours. Thereafter, water was added to the reaction solution, and the mixed solution was then extracted with dichloromethane. The organic layer thus obtained was dried over anhydrous sodium sulfate. The solvent was distilled away under reduced pressure to obtain the title compound (429 mg, yield: 98%).

WORKUP

后处理

  1. customthe mixture thus obtained
  2. extractionthe mixed solution was then extracted with dichloromethane
  3. customThe organic layer thus obtained
  4. dry with materialwas dried over anhydrous sodium sulfate
  5. distillationThe solvent was distilled away under reduced pressure