Piperazine → 4-Chlorobenzhydrol

HRID 497140

反応式

HRID 497140 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8](Cl)[C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[CH:4][CH:3]=1.N1CCNCC1.C([O-])([O-])=[O:23].[K+].[K+]>CC(=O)CC>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[OH:23])=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 4837PiperazineHCID 11430Potassium CarbonateHCID 2415844-Chlorobenzhydryl chloride

生成物 1

HCID 84014-Chlorobenzhydrol収率 57%

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

A mixture of 1-chloro-4-(chloro-phenyl-methyl)-benzene (4.12 g, 17.4 mmol) in butanone (20 ml), anhydrous piperazine (5.98 g, 69.6 mmol), anhydrous K2CO3 (2.40 g, 17.4 mmol) and KI (2.88 g, 17.4 mmol) was refluxed under nitrogen for 18 hours. The mixture was then cooled and filtered and the solvent removed in vacuo. The residue was dissolved in CH2Cl2 (100 ml) and washed with water (30 ml). Drying and removal of the solvent followed by chromatography (CH2Cl2:CH3OH:NH4OH 90:10:0.5) afforded desired product in 57% yield. D. Synthesis of 1-{4-[(4-Chloro-phenyl)-phenyl-methyl]-piperazin-1-yl}-3,3-diphenyl-propan-1-one

後処理

  1. temperaturewas refluxed under nitrogen for 18 hours
  2. temperatureThe mixture was then cooled
  3. filtrationfiltered
  4. customthe solvent removed in vacuo
  5. dissolutionThe residue was dissolved in CH2Cl2 (100 ml)
  6. washwashed with water (30 ml)
  7. customDrying
  8. customremoval of the solvent

出典と根拠

ORDレコード
ord-023affac69994085b27be9146dc4f795
出典データセット
uspto-grants-2005_09
特許番号
US06949554B2

関連ノート

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