Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Chloroform | HCID 6212 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | HCID 19852111 | HCID 19852111 | — |
| Reactant | Potassium tert-butoxide | HCID 23665647 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 19852517 | HCID 19852517 | — |
Reaction Steps
To 6.5 g of triphenyl phosphine and 2.5 g of potassium t-butoxide dissolved in 75 ml of THF and cooled to -70° C. was added 3.5 g of chloroform. After stiring for 5 minutes a solution of 3.9 g of N-(4-trifluoromethoxyphenyl)-3-(4-chlorophenyl)-4-formyl-4-methyl-4,5-dihydro-1H-pyrazole-1-carboxamide in 10 ml of THF is added and the mixture is allowed to warm to 10° C. over 1 hour. The resulting mixture is partitioned between ether and water, dried, rotovaped and chromatographed (ether/hexane) on silica gel yielding 3.1 g of N-(4-trifluoromethoxyphenyl)-3-(4-chlorophenyl)-4-(2,2-dichlorovinyl)-4-methyl-4,5-dihydro-1H-pyrazole-1-carboxamide mp 138°-141° C. NMR and IR data were consistent with the structure.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04863947 |
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| Source dataset | uspto-grants-1989_09 |
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| ORD ID | ord-fe55566506884cbdb4028f65db7320e3 |
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| Source note | uspto-grants-1989_09 |
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