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Diisopropylethylamine → HCID 58360481、化合物

HRID 2274554
ノート
印刷プレビュー

反応式

HRID 2274554 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 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、化合物

生成物 1

HCID 58360481HCID 58360481、化合物

試薬・触媒・溶媒 2

HCID 6228
Dimethylformamide
溶媒
HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-519159654e344c008e3a52584edbece0
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09126955B2

反応ノート

読み込み中…

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