반응 #63613

반응 방정식

N-(5-fluoro-2-methylphenyl)tetrahydro-3,3-dimethyl-3H-oxazolo[3,4-a]pyrazine-7(8H)-acetamide

hydrochloric acid

sodium carbonate

→

N-(5-fluoro-2-methylphenyl)-3-(hydroxymethyl)-1-piperazineacetamide

수율 59.4%

반응 조건

후처리

1. 1
   온도refluxed for 2 hours
2. 2
   추출The product was extracted with trichloromethane
3. 3
   세척The extract was washed with water
4. 4
   기타dried
5. 5
   여과filtered
6. 6
   기타evaporated
7. 7
   기타The residue was purified by column-chromatography over silica gel using
8. 8
   workup.ADDITIONa mixture of trichloromethane and methanol
9. 9
   기타The pure fractions were collected
10. 10
    기타the eluent was evaporated
11. 11
    기타The residue was triturated in 2,2'-oxybispropane
12. 12
    여과The product was filtered off
13. 13
    기타dried

실험 절차

A mixture of 8.5 parts of N-(5-fluoro-2-methylphenyl)tetrahydro-3,3-dimethyl-3H-oxazolo[3,4-a]pyrazine-7(8H)-acetamide and 105.6 parts of hydrochloric acid solution 0.5N was stirred and refluxed for 2 hours. The reaction mixture was cooled to room temperature. The whole was alkalized with sodium carbonate and salted out. The product was extracted with trichloromethane. The extract was washed with water, dried, filtered and evaporated. The residue was purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol, saturated with ammonia (85:15 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was triturated in 2,2'-oxybispropane. The product was filtered off and dried, yielding 4.4 parts (59.4%) of N-(5-fluoro-2-methylphenyl)-3-(hydroxymethyl)-1-piperazineacetamide; mp. 127.7° C. (intermediate 145).

출처