تفاعل #737464

معادلة التفاعل

2,3-epoxy-indane

pyrrolidine

sodium chloride

sodium hydroxide

→

2,3-dihydro-1-(1-pyrrolidinyl)-1H inden-2-ol

المذيبات

water

water

ظروف التفاعل

المعالجة

1. 1
   أخرىrose to 65° C.
2. 2
   workup.ADDITIONwere added when the reaction
3. 3
   workup.DISTILLATIONExcess pyrrolidine was distilled off under reduced pressure
4. 4
   أخرىto obtain an oily phase
5. 5
   استخلاصExtraction
6. 6
   أخرىafter drying
7. 7
   تركيزconcentrating
8. 8
   workup.DISTILLATIONby distilling under reduced pressure
9. 9
   أخرىthe oil obtained
10. 10
    أخرىwas purified by chromatography over silica (eluent:ethyl acetate with 5% of triethylamine)

الإجراء التجريبي

10.8 ml of pyrrolidine in 6.75 g of 2,3-epoxy-indane [described by Mousseron et al. Bulletin de la, Societe Chimique de France, 1946, p. 629-630] in 10.8 ml of demineralized water. The temperature rose to 65° C. and the solution was stirred for 90 minutes at this temperature and 20 ml of demineralized water were added when the reaction was finished. Excess pyrrolidine was distilled off under reduced pressure to obtain an oily phase and an aqueous phase. These are saturated with sodium chloride at 20° C. and 1 ml of 32% sodium hydroxide was added. Extraction was done with ether and after drying and concentrating by distilling under reduced pressure, the oil obtained was purified by chromatography over silica (eluent:ethyl acetate with 5% of triethylamine) to obtain 8.31 g of [trans (±)] 2,3-dihydro-1-(1-pyrrolidinyl)-1H inden-2-ol.

المصدر