HRID499163

反应详情

EQUATION

反应方程式

HRID 499163 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1-(2-chloroethyl)-3-{6-[4-(2-trifluoromethylbenzoyl)piperazin-1-yl]-pyridazin-3-yl}urea (0.296 g, 0.650 mmol), potassium hydroxide (0.364 g, 0.650 mmol), in BuOH (20 mL) was refluxed overnight. The reaction mixture was concentrated and purified by column chromatography. The title compound was obtained as a light yellow powder in 71% yield (0.213 g). 1H NMR (300 MHz, CDCl3) δ 8.43 (d, J=9.9 Hz, 1H), 7.72 (d, J=7.8 Hz, 1H), 7.48-1.64 (m, 2H), 7.34 (d, J=7.5 Hz, 1H), 7.01 (d, J=9.9 Hz, 1H), 4.91-5.12 (br., 1H), 4.22 (t, J=7.8 Hz, 1H), 3.82-4.03 (m, 2H), 3.43-3.65 (m, 6H), 3.31 (t, J=5.7 Hz, 2H).

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated
  2. custompurified by column chromatography