Methylamine → 2,4-Dihydro-5-methoxy-4-methyl-3H-1,2,4-triazol-3-one

Temperature

70 °C

8.11 g (0.05 mol) of methyl N′-dimethoxymethylenehydrazinecarboxylate were dissolved in 25.4 g of methanol and admixed with 3.26 g (0.105 mol) of methylamine, dissolved in methanol, and the mixture was heated in an autoclave at 70° C. for 14 hours. The reaction mixture was concentrated under reduced pressure and taken up in water (10 ml). The mixture was acidified by addition of conc. HCl. The crystals which precipitated at 4° C. were filtered off and dried. This gave 1.89 g (29.3%) of 5-methoxy-4-methyl-2,4-dihydro-1,2,4-triazol-3-one in the form of a colourless solid. Melting point 146-148° C.

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. additionThe mixture was acidified by addition of conc. HCl
3. customThe crystals which precipitated at 4° C.
4. filtrationwere filtered off
5. customdried

ORD record

ord-03288de3d1a74ba8ad443b15b9fdc0f6

Source dataset

uspto-grants-2001_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06248900B1