HRID75816

反应详情

EQUATION

反应方程式

HRID 75816 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. extractionextracted with EtOAc
  2. customOrganic layer was separated
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated under reduced pressure
  5. customto get off white solid, which
  6. customwas crystallized from CH2Cl2