تفاعل #93187

ord-2623fdde1a7947069d7976ff1131d293

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    تجفيفdrying of the organic phase with magnesium sulpate, filtration, evaporation and recrystallisation from ethyl acetate

الإجراء التجريبي

6-Cyano-3,4-dihydro-2,2-dimethyl-3,4-epoxy-2H-benzo[b]pyran and 2-piperidone were stirred in dimethyl sulphoxide under nitrogen at room temperature. Sodium hydride (81% dispersion in mineral oil) was added during 5 mins. and the reaction stirred for a further 6 hours. Addition of water, extraction with ethyl acetate, drying of the organic phase with magnesium sulpate, filtration, evaporation and recrystallisation from ethyl acetate gave 6-cyano-3,4-dihydro-2,2-dimethyl-trans-4-(2-oxo-1-piperidinyl)-2H-benzo[b]pyran-3-ol was prepared, as crystals of m.p. 155° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04610992uspto-grants-1986_09