1-Butanol → 4-(4-Amino-phenyl)-1-methyl-1H-pyrazolo[3,4-c]pyridin-3-ylamine

HRID 1159451Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1159451
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:15]=[N:14][CH:13]=C(Cl)[C:9]=2[C:10]#[N:11])=[CH:4][CH:3]=1.[CH3:17][NH:18][NH2:19].[CH2:20](O)CCC>>[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[CH:15]=[N:14][CH:13]=[C:17]3[N:18]([CH3:20])[N:19]=[C:10]([NH2:11])[C:9]=23)=[CH:6][CH:7]=1

Komponenten

4

Versuchsvorschrift

The product from Example 1C (150 mg, 0.65 mmol) and methylhydrazine (0.35 mL) in n-butanol (2 mL) was heated in a sealed vial at 190° C. for 30 minutes with stirring in a Smith Synthesizer microwave oven (at 300W). The reaction mixture was allowed to cool to room temperature and partitioned between water and ethyl acetate. The organic extract was dried (Na2SO4), filtered, and the filtrate was concentrated to provide 0.08 g of the title compound. MS (ESI(+)) m/e 240 (M+H)+.

Aufarbeitung

  1. custompartitioned between water and ethyl acetate
  2. extractionThe organic extract
  3. dry with materialwas dried (Na2SO4)
  4. filtrationfiltered
  5. concentrationthe filtrate was concentrated

Quellen und Nachweise

ORD-Eintrag
ord-dd4d95861b45473a84a5f97180212f45
Quelldatensatz
uspto-grants-2010_10
Patentnummer
US07812166B2

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