Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 3-Fluoro-α-oxobenzeneacetic acid | HCID 13548098 | — |
| Reactant | HCID 21277249 | HCID 21277249 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 21277255 | HCID 21277255 | 86.3% |
Reaction Steps
3.8 g (0.02 mole) of 3-fluorophenylglyoxylic acid in 10 ml of ethanol are slowly added dropwise to a solution of 5.4 g (0.022 mole) of 1-amino-2-methyl-3-methylaminoguanidine hydroiodide in 55 ml of 2N hydrochloride acid. The temperature rises from 20° to 30° C. during this addition and a pale yellow precipitate forms. This mixture is stirred for 2 hours to a temperature in the range from 60° to 70° C., whereupon a clear yellow orange solution forms. After cooling, this solution is neutralised with an aqueous solution of sodium hydroxide. The precipitate is then isolated, washed with water and dried at 70° C., affording 4.3 g (76% of theory) of 3,4-bis(methylamino)-6-(3-fluorophenyl)-4H-1,2,4-triazin-5-one with a melting point of 173°-174° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04801708 |
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| Source dataset | uspto-grants-1989_01 |
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| ORD ID | ord-5009b374d7ee4555ad4df5baa4f6c2e6 |
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| Source note | uspto-grants-1989_01 |
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