Triethylamine → 4-(5-amino-6-(2-(6-aminopyridine-2-carbonyl)hydrazinecarbonyl)pyrazin-2-yl)-N,N-dimethylbenzamide

HRID 78621

Reaktionsgleichung

Reaktionsgleichung von HRID 78621
[NH2:1][C:2]1[N:3]=[CH:4][C:5]([C:12]2[CH:22]=[CH:21][C:15]([C:16]([N:18]([CH3:20])[CH3:19])=[O:17])=[CH:14][CH:13]=2)=[N:6][C:7]=1[C:8]([NH:10][NH2:11])=[O:9].[NH2:23][C:24]1[N:29]=[C:28]([C:30](O)=[O:31])[CH:27]=[CH:26][CH:25]=1.C(N(CC)CC)C.F[B-](F)(F)F.N1(OC(=[N+](C)C)N(C)C)C2C=CC=CC=2N=N1>CN(C=O)C>[NH2:1][C:2]1[N:3]=[CH:4][C:5]([C:12]2[CH:13]=[CH:14][C:15]([C:16]([N:18]([CH3:19])[CH3:20])=[O:17])=[CH:21][CH:22]=2)=[N:6][C:7]=1[C:8]([NH:10][NH:11][C:30]([C:28]1[CH:27]=[CH:26][CH:25]=[C:24]([NH2:23])[N:29]=1)=[O:31])=[O:9]

Komponenten

6

Versuchsvorschrift

A solution of 4-[5-amino-6-(hydrazinecarbonyl)pyrazin-2-yl]-N,N-dimethyl-benzamide (100 mg, 0.3163 mmol) and 6-aminopyridine-2-carboxylic acid (43.69 mg, 0.3163 mmol) in DMF (1.000 mL) was treated with triethylamine (32.01 mg, 44.09 μL, 0.3163 mmol) then warmed slightly. The mixture was cooled to room temperature and then treated with (benzotriazol-1-yloxy-dimethylamino-methylene)-dimethyl-ammonium tetrafluoroborate (121.9 mg, 0.3796 mmol) and stirred at room temperature overnight. The mixture was poured dropwise onto water (5 ml) with rapid stirring, stirred at room temperature for 1 h then filtered to give a wet paste which was dried under high vacuum at 100° C. overnight. Used directly in the next step without purification.

Aufarbeitung

  1. temperaturethen warmed slightly
  2. additionThe mixture was poured dropwise onto water (5 ml) with rapid stirring
  3. stirringstirred at room temperature for 1 h
  4. filtrationthen filtered
  5. customto give a wet paste which
  6. customwas dried under high vacuum at 100° C. overnight
  7. customUsed directly in the next step without purification

Quellen und Nachweise

ORD-Eintrag
ord-04f9d786475440d3a8e31f38bff41582
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08841308B2

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