Cyanoacetamide → HCID 13649665, Verbindung

To a stirred solution of sodium (0.147 g, 6.41 mmol) in ethanol (20 ml) under nitrogen atmosphere was added 2-cyanoacetamide (539 mg, 6.41 mmol) and the mixture was refluxed 10 minutes. The mixture was cooled slightly, 3-(4-chlorobenzoyl)-4-chlorobenzyl azide (1.51 g, 4.93 mmol) was added, and the mixture was refluxed 1 hour. The mixture was cooled to 0° C. and filtered. The product was washed with ice cold ethanol (2×5 ml), water (3×5 ml), ice cold ethanol (2×5 ml), and diethyl ether (10 ml), and dried at 50° C. for 3 hours under vacuum to provide 1.16 g (60%) of 5-amino-1-(3-[4-chlorobenzoyl]-4-chlorobenzyl)-1,2,3-triazole-4-carboxamide, m.p. 189°-192° C.

1. temperaturethe mixture was refluxed 10 minutes
2. temperatureThe mixture was cooled slightly
3. temperaturethe mixture was refluxed 1 hour
4. filtrationfiltered
5. washThe product was washed with ice cold ethanol (2×5 ml), water (3×5 ml), ice cold ethanol (2×5 ml), and diethyl ether (10 ml)
6. customdried at 50° C. for 3 hours under vacuum

ORD-Eintrag

ord-70e07a0ce3a3461da0a6d7998eb15692

Quelldatensatz

uspto-grants-1986_05

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US04590201