HRID869207

反应详情

EQUATION

反应方程式

HRID 869207 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

t-Butyl 6-chloropyridazin-3-yl((1-(3-fluoropyridin-2-yl)cyclobutyl)methyl)carbamate (900 mg, 2.29 mmol, 1 equiv), 5-cyanothiophen-2-ylboronic acid (390 mg, 2.52 mmol, 1.1 equiv), (dppf)PdCl2 (164 mg, 0.23 mmol, 0.1 equiv), nitrogen-sparged dioxane (6.0 mL) and aq. 2 N K2CO3 (2.3 mL) were combined and heated in a microwave reactor for 30 min at 140° C. The reaction mixture was filtered through a Celite plug and the filtrate was concentrated. The resulting residue was purified on silica gel using a mixture of ethyl acetate and hexanes to provide the title compound as a yellow oil (340 mg, 32%), LRMS (M+H+) m/z 466.3.

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered through a Celite plug
  2. concentrationthe filtrate was concentrated
  3. customThe resulting residue was purified on silica gel using
  4. additiona mixture of ethyl acetate and hexanes