HRID75816
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
3-{4-[3-(2-Fluoro-phenyl)ureido]-phenyl}-isoxazole-5-carboxylic acid ethyl ester (4.6 g) was dissolved in THF (92 ml). 1M aqueous NaOH solution (65 ml) was added and stirred at RT for 15-20 minutes. The reaction mixture was acidified with dilute HCl and extracted with EtOAc. Organic layer was separated, dried over Na2SO4 and concentrated under reduced pressure to get off white solid, which was crystallized from CH2Cl2 to yield 3.68 g (86%) white solid. MS (ES+): m/z 342 (M+1); 1HNMR (DMSO-d6, 300 MHz): δ 9.33 (s, 1H), 8.63 (s, 1H), 8.13 (m, 1H), 7.89 (d, 2H), 7.7 (s, 1H), 7.6 (d, 2H), 7.23 (m, 1H), 7.13 (m, 1H), 7.02 (m, 1H).
WORKUP
后处理
- extractionextracted with EtOAc
- customOrganic layer was separated
- dry with materialdried over Na2SO4
- concentrationconcentrated under reduced pressure
- customto get off white solid, which
- customwas crystallized from CH2Cl2