반응 #1621148

반응 방정식

2-(phenoxymethyl)oxirane

3-(2-ethoxyethyl)-2-(1-piperazinylmethyl)-3H-imidazo[4,5-b]pyridine

→

4-[[3-(2-ethoxyethyl)-3H-imidazo[4,5-b]pyridin-2-yl]methyl]-α-(phenoxymethyl)-1-piperazineethanol

수율 31.0%

용매

2-propanol

반응 조건

후처리

1. 1
   온도at reflux temperature
2. 2
   기타The reaction mixture was evaporated
3. 3
   기타the residue was purified by column chromatography over silica gel using
4. 4
   workup.ADDITIONa mixture of trichloromethane and methanol (95:5 by volume) as eluent
5. 5
   기타The pure fractions were collected
6. 6
   기타the eluent was evaporated
7. 7
   기타The residue was crystallized from 2,2'-oxybispropane
8. 8
   여과The product was filtered off
9. 9
   기타dried

실험 절차

A mixture of 1.65 parts of 2-(phenoxymethyl)oxirane, 8.9 parts of 3-(2-ethoxyethyl)-2-(1-piperazinylmethyl)-3H-imidazo[4,5-b]pyridine and 40 parts of 2-propanol was stirred for 20 hours at reflux temperature. The reaction mixture was evaporated and the residue was purified by column chromatography over silica gel using a mixture of trichloromethane and methanol (95:5 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was crystallized from 2,2'-oxybispropane. The product was filtered off and dried, yielding 1.36 parts (31.0%) of 4-[[3-(2-ethoxyethyl)-3H-imidazo[4,5-b]pyridin-2-yl]methyl]-α-(phenoxymethyl)-1-piperazineethanol; mp. 102.5° C. (compound 118).

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