Methylhydrazine → [8-(benzylthio)-1-methyl-4,5-dihydro-1H-pyrazolo[4,3-h]quinazolin-3-yl](phenyl)methanone

HRID 44616

Reaktionsgleichung

Reaktionsgleichung von HRID 44616
[CH2:1]([S:8][C:9]1[N:18]=[CH:17][C:16]2[CH2:15][CH2:14][CH:13]([C:19](=O)[C:20]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)=[O:21])[C:12](=O)[C:11]=2[N:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:30][NH:31][NH2:32]>C(O)C>[CH2:1]([S:8][C:9]1[N:18]=[CH:17][C:16]2[CH2:15][CH2:14][C:13]3[C:19]([C:20]([C:22]4[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=4)=[O:21])=[N:32][N:31]([CH3:30])[C:12]=3[C:11]=2[N:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Komponenten

4

Versuchsvorschrift

0.22 g (0.55 mmol) of 1-[2-(benzylthio)-8-oxo-5,6,7,8-tetrahydroquinazolin-7-yl]-2-phenylethane-1,2-dione were dissolved in 6 mL of ethanol and 0.03 g (0.66 mmol) of methyl hydrazine were added. The reaction mixture was maintained under stirring at refluxing temperature for 5 hours. After that time the solvent was removed under reduced pressure, the residue redissolved with dichloromethane and washed with water. The organic layer was dried over Na2SO4 and concentrated, giving 0.16 g of the title compound (70% yield).

Aufarbeitung

  1. temperatureThe reaction mixture was maintained
  2. temperatureat refluxing temperature for 5 hours
  3. customAfter that time the solvent was removed under reduced pressure
  4. dissolutionthe residue redissolved with dichloromethane
  5. washwashed with water
  6. dry with materialThe organic layer was dried over Na2SO4
  7. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-2f282143c0da43daa8201b53de856855
Quelldatensatz
uspto-grants-2013_09
Patentnummer
US08541429B2

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