HRID2366205
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
TFA (5 mL) was added to a solution of (2-chloro-3-fluoropyridin-4-yl)carbamic acid tert-butyl ester (1.9 g, 7.7 mmol) in DCM (10 mL). The solution was stirred at ambient temperature for 5 hours and concentrated under reduced pressure. The resultant residue was dissolved in DCM and purified by column chromatography on a NH2 cartridge (0-10% MeOH in DCM) to afford the title compound as a beige solid (0.96 g, 94% yield). 1H NMR (400 MHz, CDCl3): δ 7.82 (d, J=5.4 Hz, 1H), 6.60 (t, J=5.8 Hz, 1H), 4.38 (br s, 2H).
WORKUP
后处理
- concentrationconcentrated under reduced pressure
- dissolutionThe resultant residue was dissolved in DCM
- custompurified by column chromatography on a NH2 cartridge (0-10% MeOH in DCM)