Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | 2-Chloroaniline | HCID 7240 | — |
| Reactant | 3-(Difluoromethyl)-1-methyl-1 H-pyrazole-4-carbonyl chloride | HCID 15340110 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 66863415 | HCID 66863415 | — |
Reaction Steps
80.0 g (0.403 mol, 98% pure) of 3-difluoromethyl-1-methyl-1H-pyrazole-4-carbonyl chloride were dissolved at 25° C. in 257.2 g of toluene. The solution was evacuated to 400 mbar and heated to 85° C. Subsequently, within 3 hours, 221.3 g (0.399 mol, 23% strength) of toluenic 2-chloroaniline solution were metered in and the reaction mixture was stirred for a further 1 hour. After venting and cooling to 20° C. with a ramp of 10° C./h, the mixture was stirred overnight. Subsequently, the mixture was cooled to 0° C., and the solids were filtered off, washed with cold toluene and dried at 80° C. under reduced pressure. The yield (without further processing of the mother liquor) was 105 g (92%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08350046B2 |
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| Source dataset | uspto-grants-2013_01 |
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| ORD ID | ord-0339bc97253a4b48924b806723e7680a |
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| Source note | uspto-grants-2013_01 |
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