HuagongsheHuagongshe Chemistry Print Report · For research reference only
Thiourea → 5-(Difluoromethoxy)-1-methyl-3-(trifluoromethyl)-1H-pyrazol-4-yl-carbamimidothioic acid methyl ester hydrobromide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Thiourea | HCID 2723790 | — |
| Reactant | 4-(bromomethyl)-5-(difluoromethoxy)-1-methyl-3-(trifluoromethyl)-1H-pyrazole | HCID 11722838 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 5-(Difluoromethoxy)-1-methyl-3-(trifluoromethyl)-1H-pyrazol-4-yl-carbamimidothioic acid methyl ester hydrobromide | HCID 23075689 | 77.5% |
Reaction Steps
To a solution of 19.1 g (purity: 75.0%, 46.3 mmol) of 4-bromomethyl-5-difluoromethoxy-1-methyl-3-trifluoromethyl-1H-pyrazole in 30 ml of ethanol was added 3.5 g (46.3 mmol) of thiourea, followed by 1 hour of heating and refluxing under stirring. The solvent was removed by evaporation under reduced pressure and the residue was washed with a mixed solvent of ethyl acetate and n-hexane to obtain 13.8 g (yield: 77.5%) of 2-(5-difluoromethoxy-1-methyl-3-trifluoromethyl-1H-pyrazole-4-ylmethyl)-isothiourea hydrobromide as white crystals (melting point: 130 to 131° C.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07256298B2 |
| Source dataset | uspto-grants-2007_08 |
| ORD ID | ord-74384e3f3db14e058e054bddbf1220ed |
| Source note | uspto-grants-2007_08 |