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
To a solution of 2-[3-Methylcarbamoyl-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzoic acid methyl ester (0.20 g, 0.49 mmol) in methanol (1.4 mL) and tetrahydrofuran (0.6 mL) was added a solution of sodium hydroxide (59 mg, 1.47 mmol) in water (0.3 mL). The reaction was heated to 60 degrees Celsius for 1 hour and then was cooled to room temperature. The pH was adjusted with 2 N HCl to a pH of 2. EtOAc (30 mL) and water (30 mL) was added and the layers were separated. The aqueous was extracted with EtOAc (3×20 mL) and the organic layers were combined. After washing with water (15 mL), the organic layer was dried over Na2SO4. The solids were filtered away, and the organic was evaporated to yield a yellow solid (193 mg, 100%).
WORKUP
后处理
- temperatureThe reaction was heated to 60 degrees Celsius for 1 hour
- customthe layers were separated
- extractionThe aqueous was extracted with EtOAc (3×20 mL)
- washAfter washing with water (15 mL)
- dry with materialthe organic layer was dried over Na2SO4
- filtrationThe solids were filtered away
- customthe organic was evaporated