Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Toluene | HCID 1140 | — |
| Reactant | Lawesson's reagent | HCID 87949 | — |
| Reactant | HCID 21712164 | HCID 21712164 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 21712145 | HCID 21712145 | 61.6% |
Reaction Steps
0.50 g of 1-benzyl-3-chloro-6-(4-chloro-5-difluoromethoxy-1-methyl-[1H]-pyrazol-3-yl)-5-fluoro-[1H]-pyridin-2-one is introduced into 5 ml of toluene, 0.63 g of Lawesson's reagent is added and the resulting yellow suspension is stirred overnight at 120° C. The next day, the mixture is cooled to 22° C., diluted with methylene chloride and, after the addition of 3 g of silica gel, concentrated to dryness in vacuo. The silica gel is applied to a flash chromatography column and eluted first with toluene/ethyl acetate 30/1 (v/v) and then with n-hexane/ethyl acetate 2/1 (v/v). 0.32 g of the desired title compound is obtained in the form of a yellow solid having a melting point of 135-138° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06274536B1 |
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| Source dataset | uspto-grants-2001_08 |
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| ORD ID | ord-6e33a53eafe8469d82c7a10cd1049adc |
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| Source note | uspto-grants-2001_08 |
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