HRID2105053
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- -78 °C
PROCEDURE
实验过程
To a solution of 1-methyl-3-phenyl-1H-1,2,4-triazole (284 mg, 1.8 mmol, see J. Chem. Soc., 1954, 3319-3322) in THF (112 mL) at −78° C. was added BuLi (1.15 mL, 1.6 M in hexanes, 1.8 mmol). The reaction was stirred for 5 minutes at -78° C. and a solution of intermediate 370.1 (200 mg, 1.5 mmol) in THF (2 mL) was added dropwise. The mixture was warmed to ambient temperature over 2 h. Ammonium chloride (80 mg) was added to the mixture and it was concentrated. Purification of the crude material afforded 350 mg of intermediate 370.2 as a white solid. LCMS 294.2 (M+H)+.
WORKUP
后处理
- temperatureThe mixture was warmed to ambient temperature over 2 h
- concentrationwas concentrated
- customPurification of the crude material