Dimethylformamide → 4-(Diphenylmethyl)-1-piperazineethanol

HRID 746241

反応式

HRID 746241 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 47425734-(Diphenylmethyl)-1-piperazineethanol収率 84.4%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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)]

出典と根拠

ORDレコード
ord-a7f89949a20b48bfbffc559b3f3b5a68
出典データセット
uspto-grants-1986_07
特許番号
US04603135

関連ノート

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