HRID219282

反应详情

EQUATION

反应方程式

HRID 219282 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To a solution of 2,3-difluoro-5-(1-(2-(tetrahydro-2H-pyran-2-yloxy)ethyl)-1H-pyrazol-4-yl)pyridine (3.0 g, 9.5 mmol) in IPA (47.7 mL, 0.2 M) at room temperature was added hydrazine (3.6 mL, 114.4 mmol). The reaction mixture was stirred at 60° C. for 2 h, at which point the reaction was cooled to room temperature and concentrated in vacuo. The concentrated material was suspended in saturated NaHCO3 solution and filtered to obtain product as a white, fluffy solid. The material was re-suspended in water (30 mL), filtered, and dried under high vacuum to obtain 1-(3-fluoro-5-(1-(2-(tetrahydro-2H-pyran-2-yloxy)ethyl)-1H-pyrazol-4-yl)pyridin-2-yl)hydrazine (2.2 g, 72% yield) as an orange solid. MS m/z=322.2 [M+1]+. Calc'd for C15H20FN5O2: 321.4.

WORKUP

后处理

  1. temperaturewas cooled to room temperature
  2. concentrationconcentrated in vacuo
  3. filtrationfiltered
  4. customto obtain product as a white, fluffy solid
  5. filtrationfiltered
  6. customdried under high vacuum