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Diisopropylethylamine → HCID 86590131, 화합물

HRID 1840518
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HRID 1840518 반응식
[CH3:1][C:2]([CH3:31])([O:4][C:5]([NH:7][C@@H:8]([CH2:12][CH2:13][CH2:14][CH:15]1[CH2:20][CH2:19][N:18]([C:21]([O:23][CH2:24][C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)=[O:22])[CH2:17][CH2:16]1)[C:9]([OH:11])=O)=[O:6])[CH3:3].Cl.[CH2:33]([CH:35]1[CH2:40][CH2:39][NH:38][CH2:37][CH2:36]1)[CH3:34].C(N(CC)C(C)C)(C)C>ClCCl.C(OCC)(=O)C>[CH3:31][C:2]([CH3:1])([O:4][C:5]([NH:7][C@H:8]([C:9]([N:38]1[CH2:39][CH2:40][CH:35]([CH2:33][CH3:34])[CH2:36][CH2:37]1)=[O:11])[CH2:12][CH2:13][CH2:14][CH:15]1[CH2:16][CH2:17][N:18]([C:21]([O:23][CH2:24][C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)=[O:22])[CH2:19][CH2:20]1)=[O:6])[CH3:3]
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참가 물질

6

반응물 3

HCID 81531DiisopropylethylamineHCID 234481304-Ethylpiperidine hydrochlorideHCID 69820413HCID 69820413, 화합물

생성물 1

HCID 86590131HCID 86590131, 화합물수율 95%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8857Ethyl Acetate
용매

실험 절차

1.7 g (4.4 mmol) of O-(benzotriazol-1-yl)-N,N,N,N′-tetramethyluronium hexafluorophosphate (HBTU) are added portionwise, at 0° C. under nitrogen, to a solution of 1.73 g (4.0 mmol) of (S)-α-[[(1,1-dimethylethoxy)carbonyl]amino]-1-[(phenylmethoxy)carbonyl]-piperidine-4-pentanoic acid, 0.66 g (4.4 mmol) of 4-ethylpiperidine hydrochloride and 1.8 ml (10.4 mmol) of N,N-diisopropylethylamine (DIEA) in dichloromethane. The reaction mixture is allowed to warm slowly to room temperature and the reaction is continued for 18 hours. The reaction mixture is then taken up in 200 ml of ethyl acetate and is washed with 100 ml of 1N hydrochloric acid solution and then with 100 ml of saturated sodium hydrogen carbonate solution and with 100 ml of saturated sodium chloride solution. The resulting product is dried over sodium sulphate and is filtered and then concentrated. The residue obtained is purified by chromatography on a column of silica gel, eluting under pressure with a 4/6 ethyl acetate/cyclohexane mixture. 2 g of phenylmethyl (S)-4-[4-[[(1,1-dimethylethoxy)carbonyl]amino]-5-(4-ethylpiperid-1-yl)-5-oxopentyl]piperidine-1-carboxylate are obtained in the form of a viscous oil.

후처리

  1. washis washed with 100 ml of 1N hydrochloric acid solution
  2. dry with materialThe resulting product is dried over sodium sulphate
  3. filtrationis filtered
  4. concentrationconcentrated
  5. customThe residue obtained
  6. customis purified by chromatography on a column of silica gel
  7. washeluting under pressure with a 4/6 ethyl acetate/cyclohexane mixture

출처 및 근거

ORD 기록
ord-f5ae52aabbe9478288dd1539f94be35a
출처 데이터셋
uspto-grants-2004_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06680329B2

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