HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethyl Sulfate → HCID 11357876, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethyl Sulfate | HCID 6497 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | 3-(4-chloro-2-fluorophenyl)-5-difluoromethoxy-1H-pyrazole | HCID 178505826 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 11357876 | HCID 11357876 | 92.5% |
Reaction Steps
11.6 g of the 3-(4-chloro-2-fluorophenyl)-5-difluoromethoxy-1H-pyrazole (purity 86%) obtained in step 1.2 were initially charged in 100 ml of toluene. 6.2 g of dimethyl sulfate were added dropwise, and the mixture was heated at reflux for 3 h. After cooling, 25 ml of saturated aqueous NH4Cl solution were added, the mixture was stirred for 1 h and the organic phase was separated off and washed with water until neutral. Drying over Na2SO4 and concentration gave 11.3 g of 3-(4-chloro-2-fluorophenyl)-5-difluoromethoxy-1-methyl-1H-pyrazole as an oil of a purity of 82.4% (GC). Yield: 88.6%
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06897322B2 |
| Source dataset | uspto-grants-2005_05 |
| ORD ID | ord-281d408c6d9f4d0eb2192145ed3d1142 |
| Source note | uspto-grants-2005_05 |