HRID879369

反应详情

EQUATION

反应方程式

HRID 879369 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

To a stirred solution of (S)-ethyl 2-tert-butoxy-2-(7-(4-chlorophenyl)-2-(2-(1,2-dimethyl-3-oxo-2,3-dihydro-1H-indazol-6-yl)pyridin-4-yl)-5-methylbenzo[d]thiazol-6-yl)acetate (9.4 mg, 0.014 mmol) in THF (0.5 mL) and methanol (0.5 mL) was added 1N NaOH solution (0.5 mL, excess). The reaction mixture was stirred at 50° C. for 2 h and then purified by reverse phase HPLC, eluting by 0-100% acetonitrile in H2O with 0.1% TFA to give the desired product. LCMS-ESI+ (m/z): [M+H]+ calcd for C34H32ClN4O4S: 627.2; found: 627.2. 1H NMR (400 MHz, CD3OD) δ 8.75 (d, J=5.2 Hz, 1H), 8.49 (s, 1H), 8.06 (s, 1H), 7.96 (dd, J=5.2, 1.2 Hz, 1H), 7.90 (s, 1H), 7.85 (q, J=8.4 Hz, 2H), 7.70-7.67 (m, 1H), 7.61-7.56 (m, 3H), 5.27 (s, 1H), 3.51 (s, 3H), 3.47 (s, 3H), 2.62 (s, 3H), 0.98 (s, 9H).

WORKUP

后处理

  1. custompurified by reverse phase HPLC
  2. washeluting by 0-100% acetonitrile in H2O with 0.1% TFA