HRID1353942
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
- 50 °C
PROCEDURE
实验过程
2-(5-(1H-1,2,4-Triazol-3-yl)-3-bromo-1H-indazolyl)perhydro-2H-pyran (15.05 g, 43.22 mmol), triphenylmethyl chloride (19.54 g, 70.09 mmol), and triethylamine (9.9 mL, 71.02 mmol) was taken up in pyridine (115 mL) and heated at 50° C. overnight. The reaction was quenched with methanol (10 mL), cooled to room temperature, and condensed. The brown oil was dissolved in ethyl acetate and washed with sodium bicarbonate (saturated aqueous). Upon sonication in a ultrasonic bath a white to yellow precipitate formed that was filtered and washed with 10% ethyl acetate in hexanes. The precipitate was dried in a vacuum oven overnight (23.80 g, 93% yield): ES-MS (m/z) 590 [M+1]+.
WORKUP
后处理
- customThe reaction was quenched with methanol (10 mL)
- temperaturecooled to room temperature
- customcondensed
- washwashed with sodium bicarbonate (saturated aqueous)
- customUpon sonication in a ultrasonic bath a white to yellow precipitate
- customformed
- filtrationthat was filtered
- washwashed with 10% ethyl acetate in hexanes
- customThe precipitate was dried in a vacuum oven overnight (23.80 g, 93% yield)