HRID870698

反应详情

EQUATION

反应方程式

HRID 870698 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

A mixture of (3-bromo-7-methyl-imidazo[1,2-b]pyridazin-6-yl)-butyl-amine (115 mg, 0.41 mmol), (4-aminomethylphenyl)boronic acid hydrochloride (99.9 mg, 0.53 mmol), K2CO3 (170 mg, 1.23 mmol) and dichlorobis(triphenylphosphine)palladium(II) (14.4 mg, 0.021 mmol) in MeCN/water (3.2 ml/0.8 ml) was heated in a microwave at 150° C. for 15 min. The reaction mixture was diluted with MeCN and filtered. The filtrate was subjected to preparative HPLC to give the titled compound as AcOH salt (66.5 mg). 1H NMR (400 MHz, METHANOL-d4) δ ppm 1.01 (t, J=7.39 Hz, 3H) 1.42-1.52 (m, 2H) 1.73 (t, J=7.28 Hz, 2H) 2.23 (s, 3H) 3.41 (t, J=7.28 Hz, 2H) 4.16 (s, 2H) 7.44 (s, 1H) 7.52 (d, J=8.38 Hz, 2H) 7.75 (s, 1H) 8.25 (d, J=8.38 Hz, 2H) 8.54 (s, 1H). LRMS (ESI) m/z 310.2 [(M+H)]+, calc'd for C18H23N5: 309.42.

WORKUP

后处理

  1. filtrationfiltered