HRID1880394
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 methyl 3-methyl-1-[(trifluoromethyl)sulfonyl]-1H-indazole-6-carboxylate (590 mg, 1.83 mmol) in methanol/water (3:1, 72 mL) was added K2CO3 (1.01 g, 7.31 mmol) and the mixture was heated at reflux for 2 hours. The reaction was cooled to room temperature and the methanol was removed under reduced pressure. The aqueous solution was acidified to pH 3-3.5 with KHSO4. The solid was isolated by filtration, dissolved in EtOAc and washed with water. The organic layer was dried over Na2SO4, filtered and concentrated to provide the title compound (259 mg, 80%).
WORKUP
后处理
- temperaturethe mixture was heated
- temperatureat reflux for 2 hours
- customthe methanol was removed under reduced pressure
- customThe solid was isolated by filtration
- washwashed with water
- dry with materialThe organic layer was dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated