HRID1676255

反应详情

EQUATION

反应方程式

HRID 1676255 的结构方程式

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

Prepared from 1-ethyl-4-(prop -2-ynyl)piperazine (59 mg, 0.39 mmol) and 3-fluoro-4-(2-iodothieno[3,2-b]pyridin-7-yloxy)benzenamine (Example 6, Step A; 100 mg, 0.26 mmol) according to the procedure described for Example 6, Step B, except the reaction was heated at 50° C. for 7 hours. The crude was purified by preparative TLC [5% MeOH (containing 7N NH3) in CH2Cl2]. The product was obtained as a waxy solid (48 mg, 40%). 1H NMR (400 MHz, CDCl3) δ 8.47 (d, J=6 Hz, 1H), 7.58 (s, 1H), 7.03 (t, J=9 Hz, 1H), 6.53 (m, 2H), 6.47 (m, 1H), 3.86 (br s, 2H), 3.60 (s, 2H), 2.45-2.74 (m, 8H), 2.46 (q, J=7 Hz, 2H), 1.11 (t, J=7 Hz, 3H).

WORKUP

后处理

  1. customThe crude was purified by preparative TLC [5% MeOH (containing 7N NH3) in CH2Cl2]