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Diisopropylethylamine → HCID 86656441, 화합물

HRID 69911
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HRID 69911 반응식
[C:1]([O:5][C:6]([NH:8][C@H:9]1[CH2:14][NH:13][CH2:12][C@@H:11]([C:15]([OH:17])=[O:16])[CH2:10]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].CCN(C(C)C)C(C)C.[CH2:27]([O:34][C:35](ON1C(=O)CCC1=O)=[O:36])[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1>ClCCl>[CH2:27]([O:34][C:35]([N:13]1[CH2:14][C@H:9]([NH:8][C:6]([O:5][C:1]([CH3:4])([CH3:2])[CH3:3])=[O:7])[CH2:10][C@H:11]([C:15]([OH:17])=[O:16])[CH2:12]1)=[O:36])[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 83172Benzyl succinimido carbonateHCID 71601477HCID 71601477, 화합물

생성물 1

HCID 86656441HCID 86656441, 화합물수율 99%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of cis-(+/−)-5-(tert-butoxycarbonylamino)piperidine-3-carboxylic acid (1.0 eq.) in dichloromethane (0.2 M) was added DIEA (1.1 eq.), followed by N-(benzyloxycarbonyloxy)succinimide (1.0 eq.); the reaction was stirred at r.t. overnight. The solvent was removed under reduced pressure. To the crude was added EtOAc and 1N HCl. After extraction, the organic layer was washed with brine, dried and filtered, and concentrated to yield cis-(+/−)-1-(benzyloxycarbonyl)-5-(tert-butoxycarbonylamino)piperidine-3-carboxylic acid (99% yield) LCMS (m/z): 379.2 (MH+); LC Rt=3.55 min.

후처리

  1. customThe solvent was removed under reduced pressure
  2. additionTo the crude was added EtOAc and 1N HCl
  3. extractionAfter extraction
  4. washthe organic layer was washed with brine
  5. customdried
  6. filtrationfiltered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-48002924cb2a4f9fab865d979b221acd
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08822497B2

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