HRID606092

反应详情

EQUATION

反应方程式

HRID 606092 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of 1-{[3-(4-fluorophenyl)isoxazol-5-yl]methyl}-N,N-bis(4-methoxybenzyl)-6,7-dimethyl-1H-imidazo[4,5-c]pyridin-4-amine (2.0 g, 3.5 mmol) in trifluoroacetic acid (20 mL) was stirred at room temperature for 16 hours. The trifluoroacetic acid was removed under reduced pressure, and the residue was triturated with aqueous hydrochloric acid (25 mL of 6 N) and ethanol (20 mL) for 30 minutes. The resulting mixture was adjusted to pH 14 with the addition of 50% (w/w) aqueous sodium hydroxide and stirred at 0° C. for 30 minutes. A solid was present and was isolated by filtration and purified by column chromatography on silica gel (eluting with 5% to 10% CMA in chloroform). The resulting solid was dried under high vacuum at 100° C. for 18 hours to provide 0.708 g of 1-{[3-(4-fluorophenyl)isoxazol-5-yl]methyl}-6,7-dimethyl-1H-imidazo[4,5-c]pyridin-4-amine as a white powder, mp 244.0-246.0° C.

WORKUP

后处理

  1. customThe trifluoroacetic acid was removed under reduced pressure
  2. customthe residue was triturated with aqueous hydrochloric acid (25 mL of 6 N) and ethanol (20 mL) for 30 minutes
  3. additionThe resulting mixture was adjusted to pH 14 with the addition of 50% (w/w) aqueous sodium hydroxide
  4. customwas isolated by filtration
  5. custompurified by column chromatography on silica gel (eluting with 5% to 10% CMA in chloroform)
  6. customThe resulting solid was dried under high vacuum at 100° C. for 18 hours