反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customto give a solution
- washA line wash of tetrahydrofuran (50.3 mL)
- additionwas then added
- 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
- washA line wash of tetrahydrofuran (25.1 mL)
- additionwas then added
- temperaturethe solution warmed to 20° C
- addition1-Butanol (100.6 mL) was added
- customthe layers separated
- customThe separated organic layer can be evaporated to dryness