HRID1053936

反应详情

EQUATION

反应方程式

HRID 1053936 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2,5-dichloro-N-(6-methoxyhexahydrofuro[3,2-b]furan-3-yl)pyrimidin-4-amine (430 mg, 1.4046 mmol), DIPEA (546.7 mg, 4.23 mmol) and 1-methylpyrazol-4-amine hydrochloride (283.3 mg, 2.12 mmol) in n-BuOH (10 mL) was stirred in a sealed tube at 150° C. for 23 h. The reaction solution was concentrated in vacuo, and the residue was purified by silica gel column chromatography (DCM/MeOH (v/v)=50/1) to give the crude product as a white solid. The crude product was recrystallized from acetone to give the title compound as a white solid (220 mg, 42.6%).

WORKUP

后处理

  1. concentrationThe reaction solution was concentrated in vacuo
  2. customthe residue was purified by silica gel column chromatography (DCM/MeOH (v/v)=50/1)
  3. customto give the crude product as a white solid
  4. customThe crude product was recrystallized from acetone