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

HRID 1032292ノート

反応式

HRID 1032292 の反応式
[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

参加物

7

反応物 4

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

生成物 2

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

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-dd565b7f8f08445dba38c93306b8a538
出典データセット
uspto-grants-1990_09
特許番号
US04957916

反応ノート

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