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

Temperature

100 °C

693.6 g (94.4%) of methyl N′-dipropoxymethylenehydrazinecarboxylate (3 mol) were dissolved in 1752 g of methanol and admixed with 564.7 g (6 mol) of methylamine, dissolved in ethanol, and the mixture was heated in an autoclave at 100° C. for 20 hours. The reaction mixture was concentrated under reduced pressure, the residue was taken up in water (880 ml) the mixture was extracted with methylene chloride and the extract was concentrated under reduced pressure. The crystals which precipitated out on cooling were filtered off and dried. This gave 383 g (71.2%, content 87.6%) of 5-propoxy-4-methyl-2,4-dihydro-1,2,4-triazol-3-one in the form of a solid. Melting point: 72.5-73.5° C.

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. extractionwas extracted with methylene chloride
3. concentrationthe extract was concentrated under reduced pressure
4. customThe crystals which precipitated out
5. temperatureon cooling
6. filtrationwere filtered off
7. customdried

ORD record

ord-81b1faec81694c1a8421978126d0bfff

Source dataset

uspto-grants-2001_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06248900B1