HRID1062759

反应详情

EQUATION

反应方程式

HRID 1062759 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

An aqueous solution of sodium hydroxyde (1M, 0.91 ml) was added at room temperature to a solution of N-(4-(1,3-benzodioxol-5-yl)-3-{2-[(5-chloro-2-pyrimidinyl)oxy]ethoxy}-1-methyl-1H-pyrazol-5-yl)-N-(methylsulfonyl)methane sulfonamide (Preparation 49) (50 mg) in a mixture of methanol (1 ml) and dichloromethane (0.3 ml). After 1 h the reaction was diluted with an aqueous saturated solution of ammonium chloride (4 ml) and the mixture was extracted with dichloromethane (3*5 ml). The combined organic fractions were dried over sodium sulfate and concentrated under reduced pressure. The pale yellow oil was purified by preparative TLC (silica) eluted with dichloromethane:methanol (95:5) to yield the title compound as a colourless oil (33 mg)

WORKUP

后处理

  1. extractionthe mixture was extracted with dichloromethane (3*5 ml)
  2. dry with materialThe combined organic fractions were dried over sodium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe pale yellow oil was purified by preparative TLC (silica)
  5. washeluted with dichloromethane:methanol (95:5)