HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → 5-Chloro-3-(4-chlorophenyl)-1-phenyl-1H-pyrazole-4-carbaldehyde
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | 3-(4-Chlorophenyl)-1-phenyl-2-pyrazolin-5-one | HCID 10286088 | — |
| Product | 5-Chloro-3-(4-chlorophenyl)-1-phenyl-1H-pyrazole-4-carbaldehyde | HCID 21418360 | 99% |
Reaction Steps
At 5° to 10° 284 g of phosphorus oxytrichloride are added dropwise during a period of 90 minutes to 270 g of dimethylformamide. Stirring is carried out for 30 minutes at 15° and then 100 g of 3-p-chlorophenyl-1-phenyl-2-pyrazoline-5-one are added. Heating is carried out for 1.5 hours at 50° and for 21 hours at 70°. The product is poured on to 2 kg of ice, the pH is adjusted to 3-4 with 20 % of sodium hydroxide and the precipitate is filtered off. 5-Chloro-3-p-chlorophenyl-1-phenyl-pyrazole-4-carboxaldehyde is obtained with a yield of 99 %; F 169.5°-171° (from acetone).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04042702 |
| Source dataset | uspto-grants-1977_08 |
| ORD ID | ord-642c912b8d1c4b37811aa5e3f1620f44 |
| Source note | uspto-grants-1977_08 |