HRID1399793

反应详情

EQUATION

反应方程式

HRID 1399793 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A mixture of methyl 3-(3-chloro-2-methylbenzyl)-2-methyl-5-morpholino-3H-imidazo[4,5-b]pyridine-7-carboxylate (239 mg, 0.58 mmol) in 2N LiOH (15 mL) and THF (15 mL) was stirred at 60° C. for 5 h. It was cooled to room temperature and the precipitate was collected by filtration. It was then poured into water (100 mL) and the suspension was acidified with formic acid to pH=1. It was filtered and the solid was washed with water to afford the desired product as a gray solid (163 mg, 71%). LC/MS: MS (ES+) m/e 401 (MH+); 1H NMR (300 MHz, DMSO-d6) δ ppm 2.36 (s, 3H), 2.44 (s, 3H), 3.41 (s, 4H), 3.69 (s, 4H), 5.44 (s, 2H), 6.40 (d, J=7.5 Hz, 1H), 7.05-7.11 (m, 2H), 7.35 (d, 1H).

WORKUP

后处理

  1. temperatureIt was cooled to room temperature
  2. filtrationthe precipitate was collected by filtration
  3. additionIt was then poured into water (100 mL)
  4. filtrationIt was filtered
  5. washthe solid was washed with water