反応 #63624

反応方程式

5-chloro-1,1-diphenyl-2-pentanone

3-(aminocarbonyl)-N-(2,6-dichlorophenyl)-1-piperazineacetamide

→

3-(aminocarbonyl)-N-(2,6-dichlorophenyl)-4-(4-oxo-5,5-diphenylpentyl)-1-piperazineacetamide monohydrate

収率 3.7%

溶媒

N,N-dimethylformamide

反応条件

後処理

1. 1
   その他evaporated
2. 2
   抽出The product was extracted twice with dichloromethane
3. 3
   洗浄The combined extracts were washed with water
4. 4
   その他dried
5. 5
   ろ過filtered
6. 6
   その他evaporated
7. 7
   その他The residue was purified twice by column-chromatography over silica gel using
8. 8
   workup.ADDITIONa mixture of trichloromethane and methanol (95:5 by volume) as eluent
9. 9
   その他The pure fractions were collected
10. 10
    その他the eluent was evaporated
11. 11
    workup.WAITto stand for 10 days
12. 12
    ろ過The product was filtered off
13. 13
    その他dried at the air

実験手順

A mixture of 4.45 parts of 5-chloro-1,1-diphenyl-2-pentanone, 9.94 parts of 3-(aminocarbonyl)-N-(2,6-dichlorophenyl)-1-piperazineacetamide and 90 parts of N,N-dimethylformamide was stirred for 48 hours at 60° C. and evaporated. The residue was taken up in water and alkalized with ammonia. The product was extracted twice with dichloromethane. The combined extracts were washed with water, dried, filtered and evaporated. The residue was purified twice 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 taken up in 2,2'-oxybispropane and allowed to stand for 10 days. The product was filtered off and dried at the air, yielding 0.32 parts (3.7%) of 3-(aminocarbonyl)-N-(2,6-dichlorophenyl)-4-(4-oxo-5,5-diphenylpentyl)-1-piperazineacetamide monohydrate; mp. 91.6° C. (compound 171).

出典