HRID1802181
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 25 °C
PROCEDURE
实验过程
A mixture of methyl 2-(tert-butoxycarbonylamino)-5-fluoroisonicotinate (1.80 g, 6.66 mmol) and hydrochloric acid (6N in ether, 40 ml, 240 mmol) is stirred for 20 hours at 25° C. The solvent is evaporated and the light brown slurry is diluted with ethyl acetate, cooled to 0° C. and adjusted to pH 8 with sat. aqueous sodium carbonate solution. The organic layer is washed with brine, dried with magnesium sulfate and the solvent is removed under reduced pressure affording methyl 2-amino-5-fluoroisonicotinate (932 mg, 82.2%) as a brown waxy solid. MS: m/z=171.0 (M+H+).
WORKUP
后处理
- customThe solvent is evaporated
- additionthe light brown slurry is diluted with ethyl acetate
- temperaturecooled to 0° C.
- washThe organic layer is washed with brine
- dry with materialdried with magnesium sulfate
- customthe solvent is removed under reduced pressure