HRID909887

反应详情

EQUATION

反应方程式

HRID 909887 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of N-cyclohexyl-N-(2,2-dimethoxyethyl)-3-(3-(1-methyl-1H-pyrazol-4-yl)phenethoxy)propanamide (50.3 g) in tetrahydrofuran (150.9 mL) was added to a solution of p-toluenesulfonic acid monohydrate (86.3 g) in tetrahydrofuran (100.1 mL) at 20° C. to give a solution. A line wash of tetrahydrofuran (50.3 mL) was then added and the solution stirred at ambient temperature for 1 h before being added to a solution of sodium hydroxide (19.6 g) and sodium chloride (100.6 g) in water (502.9 mL) at 5° C. A line wash of tetrahydrofuran (25.1 mL) was then added and the solution warmed to 20° C. 1-Butanol (100.6 mL) was added and the layers separated. The separated organic layer can be evaporated to dryness to afford the sub-titled compound as an orange/brown oil or the solution used directly in the next Step. MS [M+H]+=398.2 (MultiMode+)

WORKUP

后处理

  1. customto give a solution
  2. washA line wash of tetrahydrofuran (50.3 mL)
  3. additionwas then added
  4. additionbefore being added to a solution of sodium hydroxide (19.6 g) and sodium chloride (100.6 g) in water (502.9 mL) at 5° C
  5. washA line wash of tetrahydrofuran (25.1 mL)
  6. additionwas then added
  7. temperaturethe solution warmed to 20° C
  8. addition1-Butanol (100.6 mL) was added
  9. customthe layers separated
  10. customThe separated organic layer can be evaporated to dryness