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1-Decylpiperazine → HCID 54231837, 화합물

HRID 1646917
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반응식

HRID 1646917 반응식
[CH2:1]([N:11]1[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10].[C:17]([O:21][C:22]([N:24]([C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)[CH2:25][C:26](O)=[O:27])=[O:23])([CH3:20])([CH3:19])[CH3:18].C(=O)([O-])O.[Na+]>CN(C)C1C=CN=CC=1.C(Cl)Cl>[C:17]([O:21][C:22]([N:24]([C:29]1[CH:30]=[CH:31][CH:32]=[CH:33][CH:34]=1)[CH2:25][C:26]([N:14]1[CH2:13][CH2:12][N:11]([CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10])[CH2:16][CH2:15]1)=[O:27])=[O:23])([CH3:20])([CH3:18])[CH3:19]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 2305441-DecylpiperazineHCID 516892Sodium BicarbonateHCID 219056362-{[(Tert-butoxy)carbonyl](phenyl)amino}acetic acid

생성물 1

HCID 54231837HCID 54231837, 화합물수율 83%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344
Dichloromethane
용매

실험 절차

A 2.3 g (8.64 mmoles) quantity of N,N,-dicyclohexylcarbodiimide was added to 20 ml of a solution of 2.0 g (7.35 mmoles) of N-decylpiperazine, 1.9 g (7.56 mmoles) of N-t-butoxycarbonylphenylglycine, 1.3 g (15.5 mmoles) of sodium hydrogen carbonate and 122 mg (1.0 mmole) of 4-dimethylaminopyridine in anhydrous methylene chloride. The mixture was stirred at room temperature for 12 hours. The precipitated crystals were collected by filtration and washed with methylene chloride. Mother liquor and the washings were concentrated under reduced pressure and the residue was purified by silica gel column chromatography (chloroform:methanol=15:1), giving 2.8 g (yield: 83%) of 1-(N-t-butoxycarbonylphenylglycyl)-4-decylpiperazine.

후처리

  1. filtrationThe precipitated crystals were collected by filtration
  2. washwashed with methylene chloride
  3. concentrationMother liquor and the washings were concentrated under reduced pressure
  4. customthe residue was purified by silica gel column chromatography (chloroform:methanol=15:1)

출처 및 근거

ORD 기록
ord-4917d928fae1439b9264199cda846c3b
출처 데이터셋
uspto-grants-1993_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05182284

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