HRID655230

反应详情

EQUATION

反应方程式

HRID 655230 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a suspension of 3-chloro-6-(1-methyl-1H-pyrazole-4-yl)-pyridazine (1.0 g, 4.81 mmol) in ethanol (20 mL) was added hydrazine monohydrate (2.33 mL, 48 mmol). The reaction mixture was stirred at 80° C. for 3.5 h, cooled to room temperature and concentrated in vacuo. The residue was triturated with 1 N aqueous potassium carbonate, filtered, washed with water and dried in vacuo to provide 2 g of the title compound as a beige solid (670 mg, 73% yield): 1H NMR (DMSO-d6) δ 3.92 (s, 3H), 4.28 (s, 1H) 7.02 (d, 1H), 7.59 (d, 1H), 7.84 (s, 1H), 7.90 (s, 1H), 8.19 (d, 1H); MS (m/z) 191 [M+H+]+.

WORKUP

后处理

  1. temperaturecooled to room temperature
  2. concentrationconcentrated in vacuo
  3. customThe residue was triturated with 1 N aqueous potassium carbonate
  4. filtrationfiltered
  5. washwashed with water
  6. customdried in vacuo