Piperazine → (2-Fluoro-phenyl)-piperazin-1-yl-methanone

HRID 1032292노트

반응식

HRID 1032292 반응식
[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.C(N(CC)CC)C.[F:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[C:21](Cl)=[N:22][NH:23][C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.C(=O)([O-])[O-:32].[K+].[K+]>ClC(Cl)Cl>[F:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[C:21]([N:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1)=[O:32].[C:24]1([NH:23][NH2:22])[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1

참가 물질

7

반응물 4

HCID 4837PiperazineHCID 8471TriethylamineHCID 11430Potassium CarbonateHCID 727453432-fluoro-N-phenylbenzenecarbohydrazonoyl chloride

생성물 2

HCID 7516PhenylhydrazineHCID 544862(2-Fluoro-phenyl)-piperazin-1-yl-methanone수율 55.8%

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

To a stirred mixture of 12.5 parts of piperazine, 3.6 parts of N,N-diethylethanamine and 75 parts of trichloromethane was added a solution of 9 parts of 2-fluoro-N-phenyl-benzenecarbohydrazonoyl chloride in 75 parts of trichloromethane. The whole was stirred for 2 hours at room temperature. After the addition of 5 parts of potassium carbonate, the reaction mixture was stirred for 30 minutes at reflux temperature. The mixture was cooled, washed with 100 parts of water and the layers were separated. The organic layer was dried, filtered and evaporated, yielding 6 parts (55.8%) of 1-(2-fluorobenzoyl)-piperazine, 2-phenylhydrazine as a residue (int. 9).

후처리

  1. stirringthe reaction mixture was stirred for 30 minutes
  2. temperatureat reflux temperature
  3. temperatureThe mixture was cooled
  4. washwashed with 100 parts of water
  5. customthe layers were separated
  6. customThe organic layer was dried
  7. filtrationfiltered
  8. customevaporated

출처 및 근거

ORD 기록
ord-dd565b7f8f08445dba38c93306b8a538
출처 데이터셋
uspto-grants-1990_09
특허 번호
US04957916

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