HuagongsheHuagongshe Chemistry Print Report · For research reference only
Difluoroacetic acid → 5-(Difluoromethyl)-2-methyl-1H-1,2,4-triazol-3(2H)-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Difluoroacetic acid | HCID 9788 | — |
| Reactant | 1-Amino-1-methylurea | HCID 256004 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | 5-(Difluoromethyl)-2-methyl-1H-1,2,4-triazol-3(2H)-one | HCID 135838251 | 36.5% |
Reaction Steps
20 ml of toluene was added to 500 mg (5.61 mmol) of 2-methyl semicarbazide (produced in the same manner as in Reference Production Example 6), and to this mixture was added 808 mg (8.41 mmol) of difluoroacetic acid, and the mixture was stirred for 10 hours under reflux with heating. The reaction solution was cooled to room temperature, then, concentrated, and the residue was subjected to silica gel thin layer chromatography (eluant: chloroform/methanol=9/1 (v/v)), to obtain 305 mg of 5-difluoromethyl-2-methyl-2,4-dihydro-3H-1,2,4-triazol-3-one having a melting point of 141.2° C. in the form of colorless solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06762197B2 |
| Source dataset | uspto-grants-2004_07 |
| ORD ID | ord-3f91772aa29f4698bb85bbd7507a48da |
| Source note | uspto-grants-2004_07 |