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Hydrochloric Acid → 3-Carbamoyl-N-(2,6-dichlorophenyl)piperazine-1-acetamide

HRID 35334
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HRID 35334 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[NH:9][C:10](=[O:24])[CH2:11][N:12]1[CH2:17][CH2:16][N:15]2C(C)(C)[NH:19][C:20](=[O:21])[CH:14]2[CH2:13]1.Cl.C(=O)([O-])[O-].[Na+].[Na+]>>[NH2:19][C:20]([CH:14]1[NH:15][CH2:16][CH2:17][N:12]([CH2:11][C:10]([NH:9][C:3]2[C:2]([Cl:1])=[CH:7][CH:6]=[CH:5][C:4]=2[Cl:8])=[O:24])[CH2:13]1)=[O:21]
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참가 물질

4

반응물 3

HCID 313Hydrochloric AcidHCID 10340Sodium CarbonateHCID 14230252N-(2,6-dichlorophenyl)hexahydro-3,3-dimethyl-1-oxoimidazo[1,5-a]pyrazine-7(1H)-acetamide

생성물 1

HCID 142302313-Carbamoyl-N-(2,6-dichlorophenyl)piperazine-1-acetamide수율 64%

실험 절차

A mixture of 23.8 parts of N-(2,6-dichlorophenyl)hexahydro-3,3-dimethyl-1-oxoimidazo[1,5-a]pyrazine-7(8H)-acetamide and 256 parts of a hydrochloric acid solution 0.5N was stirred and refluxed for 2 hours. The reaction mixture was cooled overnight to room temperature, alkalized and salted out with sodium carbonate. The product was extracted with trichloromethane. The extract was filtered and the filtrate was dried, filtered and evaporated. The residue was crystallized from acetonitrile, yielding 13.6 parts (64%) of 3-(aminocarbonyl)-N-(2,6-dichlorophenyl)-1-piperazineacetamide; mp. 180.4°-182.8° C. (intermediate 125).

후처리

  1. temperaturerefluxed for 2 hours
  2. temperatureThe reaction mixture was cooled overnight to room temperature
  3. extractionThe product was extracted with trichloromethane
  4. filtrationThe extract was filtered
  5. customthe filtrate was dried
  6. filtrationfiltered
  7. customevaporated
  8. customThe residue was crystallized from acetonitrile

출처 및 근거

ORD 기록
ord-62e55a7766674b6b9bc1d54ee3250175
출처 데이터셋
uspto-grants-1988_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04766125

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