HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → N-Methoxy-2-chloro-5-(4-chloro-5-difluoromethoxy-1-methyl-1H-pyrazol-3-yl)-4-fluorobenzamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | O-Methylhydroxylamine hydrochloride | HCID 521874 | — |
| Reactant | 2-Chloro-5-(4-chloro-5-difluoromethoxy-1-methyl-1H-pyrazol-3-yl)-4-fluorobenzoyl chloride | HCID 21254012 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | N-Methoxy-2-chloro-5-(4-chloro-5-difluoromethoxy-1-methyl-1H-pyrazol-3-yl)-4-fluorobenzamide | HCID 21254033 | — |
Reaction Steps
A solution of 8.4 g (22 mmol) of 2-chloro-5-(4-chloro-5-difluoromethoxy-1-methyl-1H-pyrazol-3-yl)-4-fluorobenzoyl chloride in 150 ml of toluene was treated with 34 g (0.24 mol) of potassium carbonate, and 16 g (48 mmol) of a 25% strength aqueous methoxyamine hydrochloride solution was subsequently added dropwise. After the reaction mixture had been stirred for 4 hours, it was diluted with 0.5 l of water. The organic phase was then separated off, washed with saturated aqueous sodium chloride solution, dried over magnesium sulfate and finally concentrated. Yield: 8.3 g.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06197973B1 |
| Source dataset | uspto-grants-2001_03 |
| ORD ID | ord-e3d96856ada84d328de40eb23164b60e |
| Source note | uspto-grants-2001_03 |