反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 20 °C
PROCEDURE
实验过程
To a stirred solution of methyl 3-(4-(N-isobutyl-N-(2-methyl-5-(trifluoromethyl)phenyl)sulfamoyl)phenyl)propanoate (15 mg, 0.033 mmol) in tetrahydrofuran (THF) (1.5 mL) at room temperature, was added a solution of lithium hydroxide (approximately 0.785 mg, 0.033 mmol—tip of spatula used) in water (1.5 mL). The reaction mixture was stirred at 20° C. for 4 hours and then stood overnight. The mixture was concentrated in vacuo then partitioned between water (2 mL) and ethyl acetate (2×5 mL). The aqueous layer was separated (hydrophilic frit) and acidified, then extracted with ethyl acetate (5 mL). The organic layer was separated (hydrophobic frit) and concentrated in vacuo to give required product, 2.4 mg. LCMS (M+1) 444, RT 1.25 mins.
WORKUP
后处理
- waitstood overnight
- concentrationThe mixture was concentrated in vacuo
- customthen partitioned between water (2 mL) and ethyl acetate (2×5 mL)
- customThe aqueous layer was separated (hydrophilic frit)
- extractionextracted with ethyl acetate (5 mL)
- customThe organic layer was separated (hydrophobic frit)
- concentrationconcentrated in vacuo