Water → Ethyl 4-(3-methyl-3-phenylbutyl)piperazine-1-carboxylate

HRID 704416노트

반응식

HRID 704416 반응식
Br[CH2:2][CH2:3][C:4]([CH3:12])([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)[CH3:5].[N:13]1([C:19]([O:21][CH2:22][CH3:23])=[O:20])[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]1.C(=O)([O-])[O-].[K+].[K+].O>O1CCCC1>[CH3:5][C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)([CH3:12])[CH2:3][CH2:2][N:16]1[CH2:15][CH2:14][N:13]([C:19]([O:21][CH2:22][CH3:23])=[O:20])[CH2:18][CH2:17]1

참가 물질

6

반응물 4

HCID 962WaterHCID 84311-Piperazinecarboxylic acid, ethyl esterHCID 11430Potassium CarbonateHCID 244007(4-Bromo-2-methylbutan-2-yl)benzene

생성물 1

HCID 14649429Ethyl 4-(3-methyl-3-phenylbutyl)piperazine-1-carboxylate수율 81.8%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 1-bromo-3-methyl-3-phenylbutane (0.73 g), ethyl piperazinecarboxylate (0.51 g) and anhydrous potassium carbonate (0.50 g) in tetrahydrofuran (5 ml) was refluxed under heating for 36 hours. To the reaction solution was added water and the solution was extracted with ethyl acetate. After washing with a saturated aqueous solution of sodium chloride, the ethyl acetate layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure. The resultant residue was subjected to silica gel column chromatography (15 g) and elution with a hexane-ethyl acetate (2:1) mixture gave 0.80 g of ethyl 4-(3-methyl-3-phenylbutyl)piperazine-1-carboxylate.

후처리

  1. temperatureunder heating for 36 hours
  2. extractionthe solution was extracted with ethyl acetate
  3. washAfter washing with a saturated aqueous solution of sodium chloride
  4. dry with materialthe ethyl acetate layer was dried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. washThe resultant residue was subjected to silica gel column chromatography (15 g) and elution with a hexane-ethyl acetate (2:1) mixture

출처 및 근거

ORD 기록
ord-e2cbc402731c4908aa4adca5f5576059
출처 데이터셋
uspto-grants-1991_01
특허 번호
US04987132

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