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Diisopropylethylamine → HCID 58360481, 화합물

HRID 2274554
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HRID 2274554 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C@@H:9]([NH:24][C:25]([O:27][C:28]([CH3:31])([CH3:30])[CH3:29])=[O:26])[C:10]([NH:12][C@@H:13]([CH:21]([CH3:23])[CH3:22])[CH2:14][O:15][CH2:16][CH2:17][C:18]([OH:20])=O)=[O:11])=[CH:4][CH:3]=1.C1C=NC2N(O)N=NC=2C=1.C(N(CC)C(C)C)(C)C.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F>CN(C=O)C.C(Cl)Cl>[CH:21]([C@@H:13]1[NH:12][C:10](=[O:11])[C@H:9]([NH:24][C:25](=[O:26])[O:27][C:28]([CH3:29])([CH3:31])[CH3:30])[CH2:8][C:5]2=[CH:6][CH:7]=[C:2]([CH:3]=[CH:4]2)[NH:1][C:18](=[O:20])[CH2:17][CH2:16][O:15][CH2:14]1)([CH3:22])[CH3:23]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 81531DiisopropylethylamineHCID 181649HOAtHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 58360480HCID 58360480, 화합물

생성물 1

HCID 58360481HCID 58360481, 화합물

시약·촉매·용매 2

HCID 6228
Dimethylformamide
용매
HCID 6344Dichloromethane용매

실험 절차

The 3-{(S)-2-[(R)-3-(4-aminophenyl)-2-tert-butoxycarbonylaminopropionylamino]-3-methylbutoxy}propionic acid (˜225 mg) obtained as crude product in 7-1 D was dissolved in 225 ml of DMF. 70.0 mg (0.51 mmol) of HOAt, 0.26 ml (1.5 mmol) of N,N-diisopropylethylamine and 195.4 mg (0.51 mmol) of HATU were successively added to this solution, and the mixture was stirred at room temp. for 1 h. The reaction mixture was concentrated in vacuo. The residue obtained in this way was taken up in CH2Cl2, washed with sat. NaHCO3 solution, dried over MgSO4 and freed of solvent in vacuo. The ring-closed compound obtained in this way was employed crude in the next stage. Yield: 215.0 mg.

후처리

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. customThe residue obtained in this way
  3. washwashed with sat. NaHCO3 solution
  4. dry with materialdried over MgSO4
  5. customThe ring-closed compound obtained in this way

출처 및 근거

ORD 기록
ord-519159654e344c008e3a52584edbece0
출처 데이터셋
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09126955B2

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