HRID2203671
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
- 20 °C
PROCEDURE
实验过程
To an ice-cooled solution of 3-iodo-1-isopropyl-5-(3-oxatricyclo[4.1.0.02,4]heptan-7-yl)-1H-pyrazole (0.500 g, 1.52 mmol) in anhydrous tetrahydrofuran (5 mL) was added lithium triethylhydroborate (10 mL, 1 M in THF) dropwise. The reaction mixture was warmed to 20° C. After 1 h, the reaction mixture was cooled to 0° C. and diluted with saturated aqueous ammonium chloride solution (10 mL). The resulting mixture was extracted with ethyl acetate (2×10 mL). The collected organic was concentrated in vacuo. Purification by flash column chromatography (17% ethyl acetate in petroleum ether) afforded product as a colorless oil (460 mg, 91% yield).
WORKUP
后处理
- temperaturethe reaction mixture was cooled to 0° C.
- extractionThe resulting mixture was extracted with ethyl acetate (2×10 mL)
- concentrationThe collected organic was concentrated in vacuo
- customPurification by flash column chromatography (17% ethyl acetate in petroleum ether)