Methylhydrazine → HCID 14126717, Verbindung
Reaktionsgleichung
O[CH:2]=[C:3]1[C:13](=O)[C:8]2[CH:9]=[N:10][N:11]([CH3:12])[C:7]=2[CH2:6][CH2:5][CH2:4]1.[CH3:15][NH:16][NH2:17]>CO>[CH3:15][N:16]1[C:13]2[C:8]3[CH:9]=[N:10][N:11]([CH3:12])[C:7]=3[CH2:6][CH2:5][CH2:4][C:3]=2[CH:2]=[N:17]1Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
To an ice-cold solution of 4 g of 5,6,7,8-tetrahydro-5-hydroxymethylene-1-methyl-4(1H) cycloheptapyrazolone in 130 ml of methanol was added, dropwise, a solution of 1.1 ml of methylhydrazine in 20 ml of methanol and the mixture was heated at reflux for 2.5 hours. Removal of the solvent under reduced pressure left a residual dark oil. The oil was flash chromatographed (7.5% 2-propanol in methylene chloride) to give 4,5,6,7-tetrahydro-1,7-dimethyl-1H-cyclohepta[1,2-c:3,4-c']dipyrazole as a yellow crystalline solid melting at about 94°-96° C. The chromatography also gave 4,5,6-tetrahydro-2,7-dimethyl-2H-cyclohepta[1,2-c:3,4-c')]dipyrazole melting at about 119°-121° C.