HRID548892

反应详情

EQUATION

反应方程式

HRID 548892 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of [3-(3-fluoro-phenyl)-5-methyl-isoxazol-4-yl]-methanol (100 mg, 0.48 mmol) in DMF (2 mL) was added sodium hydride (55% dispersion in mineral oil, 23.2 mg, 0.53 mmol). The mixture was stirred at room temperature for 15 min. After addition of a solution of 6-chloro-1,2,4-triazolo[4,3-b]pyridazine (82 mg, 0.53 mmol) in DMF (3 mL) the mixture was stirred at room temperature overnight. Then the mixture was poured into water, extracted (ethyl acetate/water) and the organic phase was dried with sodium sulfate and concentrated. Chromatography (SiO2, heptane:ethyl acetate=100:0 to 9:1) afforded the title compound (80 mg, 51%) as a white solid. MS: m/e=326.0 [M+H]+.

WORKUP

后处理

  1. stirringwas stirred at room temperature overnight
  2. extractionextracted (ethyl acetate/water)
  3. dry with materialthe organic phase was dried with sodium sulfate
  4. concentrationconcentrated