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
PROCEDURE
实验过程
To a suspension of 60% sodium hydride (59.0 mg, 1.48 mmol) in tetrahydrofuran (8 mL) was added diethyl cyanomethylphosphonate (260 μL, 1.60 mmol) at room temperature, and the mixture was stirred for 15 min. A suspension of 5-fluoro-2-methyl-6,7-dihydrocyclopenta [e] indazol-8(2H)-one (252 mg, 1.23 mmol) in tetrahydrofuran (4 mL) was added thereto, and the mixture was stirred at room temperature for 4 hr. Saturated aqueous ammonium chloride solution was added to the reaction solution, and the mixture was diluted with ethyl acetate, washed with water and saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure. The obtained crystals were washed with diisopropyl ether to give the title compound (178 mg, yield 64%).
WORKUP
后处理
- additionwas added
- stirringthe mixture was stirred at room temperature for 4 hr
- washwashed with water and saturated brine
- dry with materialdried over anhydrous sodium sulfate
- customThe solvent was evaporated under reduced pressure
- washThe obtained crystals were washed with diisopropyl ether