Methylamine → Orf 17583
Reaktionsgleichung
[CH3:1][N:2]([CH2:4][C:5]1[O:9][C:8]([CH2:10][S:11][CH2:12][CH2:13][NH:14][C:15]2[C:19](OC)=[N:18][S:17](=[O:22])[N:16]=2)=[CH:7][CH:6]=1)[CH3:3].[CH3:23][NH2:24]>>[CH3:1][N:2]([CH2:4][C:5]1[O:9][C:8]([CH2:10][S:11][CH2:12][CH2:13][NH:14][C:15]2[C:19]([NH:24][CH3:23])=[N:18][S:17](=[O:22])[N:16]=2)=[CH:7][CH:6]=1)[CH3:3]Komponenten
3
Versuchsvorschrift
To the methanolic solution of the product of Step A that was cooled to 5° in an ice-water bath was added anhydrous methylamine for 8 minutes. The reaction mixture was stirred at ambient temperature for 17 hours, then evaporated under reduced pressure to give the product as a yellow oil that was placed on 55 g of silica gel and chromatographed using a gradient elution of methylene chloride-methanol. The appropriate fraction was evaporated, dissolved in methanol and diluted with diethyl ether to yield the title compound (2.32 g) as a solid that was dried in vacuo at ambient temperature over P2O5 for 3 hours, mp 86°-92°.
Aufarbeitung
- customevaporated under reduced pressure