Dimethylformamide → 4-(Diphenylmethyl)-1-piperazineethanol

HRID 746241

반응식

HRID 746241 반응식
[N:1]1([CH2:7][CH2:8][OH:9])[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.C(=O)([O-])[O-].[K+].[K+].CN(C)C=O.[CH:21](Br)([C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1)[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1>O>[CH:21]([N:4]1[CH2:5][CH2:6][N:1]([CH2:7][CH2:8][OH:9])[CH2:2][CH2:3]1)([C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 76771-(2-Hydroxyethyl)piperazineHCID 11430Potassium CarbonateHCID 236603Bromodiphenylmethane

생성물 1

HCID 47425734-(Diphenylmethyl)-1-piperazineethanol수율 84.4%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a mixture of 1-piperazineethanol (11.4 g), potassium carbonate powder (24.3 g) and N,N-dimethylformamide (100 ml) was added dropwise benzhydryl bromide (21.7 g). The mixture was stirred at room temperature for 2 hours, then diluted with water and extracted with ethyl ether. The ethyl ether layer was washed with saturated aquus sodium chloride and dried over sodium sulfate. The solvent was then distilled off and the residue was purified by silica gel chromatography [eluent: hexane-ethyl acetate (2:1)] to give 21.9 g (84.2%) of 4-benzhydryl-1-piperazineethanol as an oil.

후처리

  1. extractionextracted with ethyl ether
  2. washThe ethyl ether layer was washed with saturated aquus sodium chloride
  3. dry with materialdried over sodium sulfate
  4. distillationThe solvent was then distilled off
  5. customthe residue was purified by silica gel chromatography [eluent: hexane-ethyl acetate (2:1)]

출처 및 근거

ORD 기록
ord-a7f89949a20b48bfbffc559b3f3b5a68
출처 데이터셋
uspto-grants-1986_07
특허 번호
US04603135

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