Piperazine → 4-Chlorobenzhydrol

HRID 497140

반응식

HRID 497140 반응식
[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

참가 물질

5

반응물 3

HCID 4837PiperazineHCID 11430Potassium CarbonateHCID 2415844-Chlorobenzhydryl chloride

생성물 1

HCID 84014-Chlorobenzhydrol수율 57%

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

실험 절차

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

후처리

  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

출처 및 근거

ORD 기록
ord-023affac69994085b27be9146dc4f795
출처 데이터셋
uspto-grants-2005_09
특허 번호
US06949554B2

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