تفاعل #974968

معادلة التفاعل

ammonium chloride

diethyl cyanomethylphosphonate

sodium hydride

5-fluoro-2-methyl-6,7-dihydrocyclopenta [e] indazol-8(2H)-one

→

title compound

المردود 64.0%

(5-fluoro-2-methyl-6,7-dihydrocyclopenta [e] indazol-8(2H)-ylidene) acetonitrile

المردود 64.0%

المذيبات

ethyl acetate

tetrahydrofuran

tetrahydrofuran

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONwas added
2. 2
   workup.STIRRINGthe mixture was stirred at room temperature for 4 hr
3. 3
   غسيلwashed with water and saturated brine
4. 4
   تجفيفdried over anhydrous sodium sulfate
5. 5
   أخرىThe solvent was evaporated under reduced pressure
6. 6
   غسيلThe obtained crystals were washed with diisopropyl ether

الإجراء التجريبي

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%).

المصدر