HRID1432731

反应详情

EQUATION

反应方程式

HRID 1432731 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
125 °C

PROCEDURE

实验过程

In a dry 25 mL round bottom flask, 8-(1-ethyl-propyl)-6-methyl-2-trifluoromethyl-imidazo[1,2-b]pyridazine (182 mg, 0.671 mmol), 5-(5-bromo-4-chloro-thiophen-2-yl)-1-methyl-1H-[1,2,4]triazole (225 mg, 0.805 mmol), KOAc (330.2 mg, 3.36 mmol), and TBAB (217 mg, 0.671 mmol) are dissolved in NMP (3 mL). The mixture is degassed with bubbling nitrogen for 20 minutes. Then, Pd(OAc)2 (8 mg, 0.034 mmol) and TDBPP (20.4 g, 0.34 moles) are added. The reaction mixture is heated to 125° C. for 3 hours to give the title compound (125 mg, 0.267 mmol, 40%). 1H-NMR (CDCl3), δ 0.88 (t, J=7.2 Hz, 6H), 1.87 (m, 4H), 2.537 (s, 3H), 3.32 (m, 1H), 4.16 (s, 3H), 6.86 (s, 1H), 7.51 (s, 1H), 7.91 (s, 1H) ppm. ES-MS (m/z): calcd for C20H20ClF3N6S (M+H)+: 468.93; found: 469.2.

WORKUP

后处理

  1. customThe mixture is degassed with bubbling nitrogen for 20 minutes