Diisopropylethylamine → HCID 178501616, Verbindung

HRID 220149

Reaktionsgleichung

Reaktionsgleichung von HRID 220149
[F:1][C:2]([F:27])([F:26])[C:3]1[NH:7][N:6]=[C:5]([C:8]2[CH:13]=[CH:12][C:11]([C@H:14]3[CH2:19][CH2:18][C@H:17]([CH2:20][C:21](OCC)=[O:22])[CH2:16][CH2:15]3)=[CH:10][CH:9]=2)[CH:4]=1.[CH3:28][NH:29][CH2:30][C:31]([O:33][CH3:34])=[O:32].F[P-](F)(F)(F)(F)F.N1(OC(N(C)C)=[N+](C)C)C2N=CC=CC=2N=N1.C(N(C(C)C)CC)(C)C>CN(C)C=O>[CH3:28][N:29]([C:21](=[O:22])[CH2:20][C@H:17]1[CH2:16][CH2:15][C@H:14]([C:11]2[CH:12]=[CH:13][C:8]([C:5]3[NH:6][N:7]=[C:3]([C:2]([F:1])([F:26])[F:27])[CH:4]=3)=[CH:9][CH:10]=2)[CH2:19][CH2:18]1)[CH2:30][C:31]([O:33][CH3:34])=[O:32]

Komponenten

6

Edukt 4

HCID 81531DiisopropylethylamineHCID 83545Sarcosine methyl esterHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 178471761HCID 178471761, Verbindung

Produkt 1

HCID 178501616HCID 178501616, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To a 20 mL scintillation vial was added the product from Example 26B (30 mg, 0.085 mmol), methyl 2-(methylamino)acetate (10.0 mg, 0.097 mmol), and N,N-dimethylformamide (0.85 mL) followed by O-(7-azabenzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium hexafluorophosphate (39.0 mg, 0.102 mmol) and diisopropylethylamine (30 μL, 0.176 mmol). Following 4 hours of stirring, the solvent was evaporated and the residue purified over RP-HPLC to afford the title product. MS (ESI) m/z 438 [M+H]+.

Aufarbeitung

  1. customthe solvent was evaporated
  2. customthe residue purified over RP-HPLC

Quellen und Nachweise

ORD-Eintrag
ord-abaa069e4a554796a40e80690b39dfaf
Quelldatensatz
uspto-grants-2012_06
Patentnummer
US08202878B2

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