تفاعل #63624

معادلة التفاعل

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

المردود 3.7%

المذيبات

N,N-dimethylformamide

ظروف التفاعل

المعالجة

1. 1
   أخرىevaporated
2. 2
   استخلاصThe product was extracted twice with dichloromethane
3. 3
   غسيلThe combined extracts were washed with water
4. 4
   أخرىdried
5. 5
   ترشيحfiltered
6. 6
   أخرىevaporated
7. 7
   أخرىThe 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
   أخرىThe pure fractions were collected
10. 10
    أخرىthe eluent was evaporated
11. 11
    workup.WAITto stand for 10 days
12. 12
    ترشيحThe product was filtered off
13. 13
    أخرىdried at the air

الإجراء التجريبي

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).

المصدر