HRID712177

反应详情

EQUATION

反应方程式

HRID 712177 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a solution of 4,6-dibromothiazolo[5,4-c]pyridin-2-amine (1.47 g, 56.74% as per LCMS, 2.70 mmol) in 1,4-dioxane (75 mL) was added ethylisocyanate (1.30 mL, 16.25 mmol) and the resulting reaction mixture was heated to 80° C. for 16 h. The solvent was distilled off under reduced pressure and the residue was then co-distilled with hexane (twice). The solid thus obtained was stirred in hot water at 80° C. for 30 min then filtered. The solid material was purified over silica gel (100-200 M, 30-40% EtOAc-hexane) to obtain the desired product as an off-white solid (0.85 g, 82%).

WORKUP

后处理

  1. customthe resulting reaction mixture
  2. distillationThe solvent was distilled off under reduced pressure
  3. customThe solid thus obtained
  4. filtrationthen filtered
  5. customThe solid material was purified over silica gel (100-200 M, 30-40% EtOAc-hexane)