HRID2381348

反应详情

EQUATION

反应方程式

HRID 2381348 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

A solution of 2-[5-chloro-6-oxo-1-(tetrahydro-pyran-2-yl)-1,6-dihydro-pyridazin-4-yloxy]-benzonitrile (61.8 g, 0.19 mol) in methanol (370 mL) was treated with a 6N aqueous hydrochloric acid solution (185 mL). The reaction was stirred at 90° C. for 4 h and then was allowed to cool to 25° C. The reaction was diluted with water. The resulting precipitate was collected by filtration, washed with water and dried in vacuo to afford 2-(5-chloro-6-oxo-1,6-dihydro-pyridazin-4-yloxy)-benzonitrile (43.1 g, 94%); ESI-MS 248 [M+H+]; HPLC: >99% (purity). 1H-NMR (300 MHz, DMSO-d6) δ 13.63 (s, 1H), 7.96-7.99 (m, 2H), 7.71-7.77 (m, 1H), 7.37-7.45 (m, 2H).

WORKUP

后处理

  1. temperatureto cool to 25° C
  2. filtrationThe resulting precipitate was collected by filtration
  3. washwashed with water
  4. customdried in vacuo