HRID1522560

反应详情

EQUATION

反应方程式

HRID 1522560 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
105 °C

PROCEDURE

实验过程

3,5-Difluoro-4-iodopicolinonitrile (1.0 g) was combined with butan-1-ol (10 mL) and hydrazine hydrate (100%, 0.82 mL) was added. The reaction was heated at 105° C. and after 2 hours cooled to room temperature, filtered, the filter rinsed with water, and the filtrate was concentrated to give a residue. The residue was washed with water and filtered to give 6-fluoro-7-iodo-1H-pyrazolo[4,3-b]pyridin-3-amine (27) as a solid (290 mg, 28% yield). 1H NMR (400 MHz, DMSO-d6) δ ppm 8.14 (s, 1H) 5.59 (s, 2H). MS [M+H] found 279.0

WORKUP

后处理

  1. additionwas added
  2. temperaturecooled to room temperature
  3. filtrationfiltered
  4. washthe filter rinsed with water
  5. concentrationthe filtrate was concentrated
  6. customto give a residue
  7. washThe residue was washed with water
  8. filtrationfiltered