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
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
To a solution of (R)-1-methoxy-3-(7-methyl-1H-indazol-5-yl)-1-oxopropan-2-yl 4-(2-oxo-1,2-dihydroquinolin-3-yl)piperidine-1-carboxylate (1.20 g, 2.46 mmol) in methanol (10 mL) and tetrahydrofuran (10 mL) at 0° C. was added a precooled solution of lithium hydroxide monohydrate (309 mg, 3.0 equiv) in water (10 mL). After 2 h, the reaction was concentrated under high vaccuum (<25° C.). The resulting residue was dissolved in water (20 mL), cooled to 0° C., and acidified to ca. pH 2 with 1 N hydrochloric acid. The suspension was maintained at 0° C. for 1 h, filtered, and the solid washed with cold water. The resulting white solid was air dried and then dried under high vacuum overnight to give 1.04 g (89%) as a white solid. Mass spec.: 475.30 (MH)+.
WORKUP
后处理
- concentrationthe reaction was concentrated under high vaccuum (<25° C.)
- dissolutionThe resulting residue was dissolved in water (20 mL)
- temperatureThe suspension was maintained at 0° C. for 1 h
- filtrationfiltered
- washthe solid washed with cold water
- customdried
- customdried under high vacuum overnight
- customto give 1.04 g (89%) as a white solid