تفاعل #791951

ord-62780a83ae9445bd8a65afa57d7b0db7

المذيبات

ظروف التفاعل

درجة الحرارة
65°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.DISTILLATIONexcess pyrrolidine was distilled off at reduced pressure
  2. 2
    أخرىto obtain an oil phase
  3. 3
    workup.ADDITIONwas added
  4. 4
    تجفيفthe ether phase was dried
  5. 5
    أخرىevaporated to dryness under reduced pressure
  6. 6
    أخرىThe oil residue was chromatographed over silica
  7. 7
    غسيلeluted with ethyl acetate containing 5% of triethylamine

الإجراء التجريبي

A solution of 10.8 ml of pyrrolidine in 6.75 g of 2,3-epoxy-indane [described by Mousseron et al, Bull. de Soc. Chim. de France, 1946, p. 629-630] was slowly added to 10.8 ml of decentralized water and after increasing the temperature to 65° C., the mixture was stirred for 90 minutes at 65° C. 20 ml of demineralized water were then added and excess pyrrolidine was distilled off at reduced pressure to obtain an oil phase and an aqueous phase. The aqueouse phase was saturated with sodium chloride and 1 ml of 32% sodium hydroxide was added thereto. The mixture was extacted with ether and the ether phase was dried and evaporated to dryness under reduced pressure. The oil residue was chromatographed over silica and eluted with ethyl acetate containing 5% of triethylamine to obtain 8.81 g of trans (±) 2,3-dihydro-1-(pyrrolidin-1-yl)-1H-inden-2-ol.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04988727uspto-grants-1991_01