HRID2075390
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 mixture of methyl 3-fluoroisoquinoline-6-carboxylate (0.257 g, 1.25 mmol) and lithium hydroxide, monohydrate (105 mg, 2.51 mmol) in THF:MeOH:H2O (3:2:1, 4 mL) was stirred at room temperature for 3 hours. The MeOH and THF were evaporated. 5% citric acid was added, and the mixture was further acidified to pH=4 with NaHSO4. The precipitate was recovered by filtration. The filtrate was extracted with chloroform-isopropanol. The organic extracts were washed with water, brine, dried over sodium sulfate and evaporated. The solids were combined to provide the product as a white solid (1.12 g, 100%). LCMS (API-ES) m/z: 192 (M+H+).
WORKUP
后处理
- customThe MeOH and THF were evaporated
- addition5% citric acid was added
- filtrationThe precipitate was recovered by filtration
- extractionThe filtrate was extracted with chloroform-isopropanol
- washThe organic extracts were washed with water, brine
- dry with materialdried over sodium sulfate
- customevaporated