Water → HCID 20074092、化合物

HRID 704377ノート

反応式

HRID 704377 の反応式
Br[CH2:2][CH2:3][CH2:4][CH2:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.[CH2:12]([O:14][C:15]([N:17]1[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1)=[O:16])[CH3:13].C(=O)([O-])[O-].[K+].[K+].O>CC(=O)CC>[CH2:12]([O:14][C:15]([N:17]1[CH2:18][CH2:19][N:20]([CH2:2][CH2:3][CH2:4][CH2:5][C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=2)[CH2:21][CH2:22]1)=[O:16])[CH3:13]

参加物

6

反応物 4

HCID 962WaterHCID 84311-Piperazinecarboxylic acid, ethyl esterHCID 11430Potassium CarbonateHCID 2596681-Bromo-4-phenylbutane

生成物 1

HCID 20074092HCID 20074092、化合物

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒2 回

反応条件

温度
80 °C

実験手順

A solution of 2.47 g of 1-bromo-4-phenylbutane in 5 ml of 2-butanone was added to a mixture of 1.93 g of 1-ethoxycarbonylpiperazine, 1.76 g of potassium carbonate and 15 ml of 2-butanone at room temperature. After stirring at 80° C. for 12 hours, the mixture was cooled and, after addition of water, extracted with ethyl acetate. The extract was washed with water and saturated aqueous solution of sodium chloride in that order and dried over anhydrous sodium sulfate. The residue obtained after concentration under reduced pressure was purified by silica gel column chromatography (eluent:hexane-ethyl acetate=4:1) to give 1-ethoxycarbonyl-4-(4-phenylbutyl)piperazine. The compound obtained was dissolved in 20 ml of ethanol and 20 ml of 10% aqueous solution of sodium hydroxide, and the solution was stirred at 100° C. for 12 hours. After cooling, the reaction mixture was extracted with ethyl acetate, and the extract was washed with saturated aqueous solution of sodium chloride and dried over anhydrous sodium sulfate. After concentration under reduced pressure, the residue was purified by silica gel column chromatography (eluent:chloroform-methanol-25% aqueous ammonia=100:10:1) to give 1.5 g cf 1-(4-phenylbutyl)piperazine as an oil.

後処理

  1. temperaturethe mixture was cooled
  2. extractionextracted with ethyl acetate
  3. washThe extract was washed with water and saturated aqueous solution of sodium chloride in that order
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe residue obtained
  6. concentrationafter concentration under reduced pressure
  7. customwas purified by silica gel column chromatography (eluent:hexane-ethyl acetate=4:1)

出典と根拠

ORDレコード
ord-dd4da86f11634ff58705cae9a0c17266
出典データセット
uspto-grants-1991_01
特許番号
US04987132

反応ノート

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