Diisopropylethylamine → [2,2-Dimethyl-4-(3-methylamino-4-nitro-benzoyl)-piperazin-1-yl]-(1-phenyl-1H-[1,2,4]-triazol-3-yl)-methanone

HRID 334072Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 334072
FC(F)(F)C(O)=O.[CH3:8][C:9]1([CH3:28])[CH2:14][NH:13][CH2:12][CH2:11][N:10]1[C:15]([C:17]1[N:21]=[CH:20][N:19]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[N:18]=1)=[O:16].[CH3:29][NH:30][C:31]1[CH:32]=[C:33]([CH:37]=[CH:38][C:39]=1[N+:40]([O-:42])=[O:41])[C:34](O)=[O:35].CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.[B-](F)(F)(F)F.CCN(C(C)C)C(C)C>CN(C=O)C>[CH3:8][C:9]1([CH3:28])[CH2:14][N:13]([C:34](=[O:35])[C:33]2[CH:37]=[CH:38][C:39]([N+:40]([O-:42])=[O:41])=[C:31]([NH:30][CH3:29])[CH:32]=2)[CH2:12][CH2:11][N:10]1[C:15]([C:17]1[N:21]=[CH:20][N:19]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[N:18]=1)=[O:16]

Komponenten

6

Edukt 4

HCID 81531DiisopropylethylamineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 221846233-(Methylamino)-4-nitrobenzoic acidHCID 86688259(2,2-dimethyl-piperazin-1-yl)-(1-phenyl-1-H-[1,2,4]triazol-3-yl)-methanone trifluoroacetate

Produkt 1

HCID 86688294[2,2-Dimethyl-4-(3-methylamino-4-nitro-benzoyl)-piperazin-1-yl]-(1-phenyl-1H-[1,2,4]-triazol-3-yl)-methanone

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A mixture of 399 mg (1.00 mmol) (2,2-dimethyl-piperazin-1-yl)-(1-phenyl-1-H-[1,2,4]triazol-3-yl)-methanone trifluoroacetate, 196 mg (1.00 mmol) 3-methylamino-4-nitro-benzoic acid, 353 mg (1.10 mmol) TBTU and 600 μL (3.50 mmol) DIPEA in 1.00 mL DMF was stirred at RT for 1 h. The reaction mixture was poured into ice water. The precipitate was filtered off, washed with water and dried.

Aufarbeitung

  1. filtrationThe precipitate was filtered off
  2. washwashed with water
  3. customdried

Quellen und Nachweise

ORD-Eintrag
ord-f786e7b19b824260832496b5d328a140
Quelldatensatz
uspto-grants-2014_11
Patentnummer
US08883789B2

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