HRID1024448

反应详情

EQUATION

反应方程式

HRID 1024448 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of methyl 2-(5-(4-(4-tert-butylbenzamido)phenyl)thiazole-2-carboxamido)-3-methylbutanoate (110 mg) in THF (2.2 ml) was added 1 M aqueous solution of Lithium hydroxide monohydrate (0.44 ml) and the reaction mixture was stirred at RT for 4 hours. The reaction mixture was acidified with dilute HCl and extracted with EtOAc. The organic layer was separated, dried over Na2SO4, concentrated under vacuum to get off white solid which was crystallized in EtOAc to give the title compound. Yield: 87 mg (81%); 1H NMR (DMSO-d6, 300 MHz): δ 13.02 (bs, 1H), 10.38 (s, 1H), 8.4 (s, 1H), 8.36 (d, 1H), 7.94 (d, 2H), 7.91 (d, 2H), 7.8 (d, 2H), 7.58 (d, 2H), 4.32 (m, 1H), 2.26 (m, 1H), 0.95 (d, 6H); MS (ES+) m/z 480 (M+1).

WORKUP

后处理

  1. extractionextracted with EtOAc
  2. customThe organic layer was separated
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated under vacuum
  5. customto get off white solid which
  6. customwas crystallized in EtOAc