Methylamine → 2,4-Dihydro-4-methyl-5-propoxy-3H-1,2,4-triazol-3-one
Reaction equation
[CH2:1]([O:4][C:5](OCCC)=[N:6][NH:7][C:8]([O:10]C)=O)[CH2:2][CH3:3].[CH3:16][NH2:17]>CO>[CH2:1]([O:4][C:5]1[N:17]([CH3:16])[C:8](=[O:10])[NH:7][N:6]=1)[CH2:2][CH3:3]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
In an autoclave, 10.02 g (44.3 mmol) of methyl N′-dipropoxymethylenehydrazinecarboxylate, 3.94 g of 39% strength solution of methylamine (49.9 mmol) in methanol and 46 g of methanol were initially charged. After 3 hours at 150° C., the solvent was distilled off. The crude substance was taken up in water (20 ml) and extracted repeatedly with methylene chloride. The organic solution was concentrated, giving 6.48 g of 5-propoxy-4-methyl-2,4-dihydro-1,2,4-triazol-3-one with a content of 50%, which corresponds to a yield of 46%.
Workup
- distillationthe solvent was distilled off
- extractionextracted repeatedly with methylene chloride
- concentrationThe organic solution was concentrated
Sources & evidence
- ORD record
- ord-0086283af23f48e9b8e64c17555b43ea
- Source dataset
- uspto-grants-2001_06
- Patent number
- US06248900B1
Reaction notes
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