HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Carbonate → 5-Chloro-1,3-dimethyl-1h-pyrazole-4-carbonyl chloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | Chlorine | HCID 24526 | — |
| Reactant | 5-Chloro-1,3-dimethylpyrazole-4-carboxaldehyde | HCID 2777397 | — |
| Solvent | Chlorobenzene | HCID 7964 | — |
| Product | 5-Chloro-1,3-dimethyl-1h-pyrazole-4-carbonyl chloride | HCID 11745492 | 74% |
Reaction Steps
To a solution of 48.5 g of 5-chloro-1,3-dimethyl-1H-pyrazole-4-carbaldehyde in 230 ml of chlorobenzene are added 36 g of sodium carbonate. Subsequently, 3.9 g of 2,2-azoisobutyronitrile (AIBN) are added at 60° C., and, within 4 hours, 24 g of chlorine gas are introduced and a further 6 g of AIBN are added. After the gas introduction has ended, the reaction solution is stirred for a further 30 minutes. The solid is filtered off and washed with a little chlorobenzene. After the solvent has been removed, 5-chloro-1,3-dimethyl-1H-pyrazole-4-carbonyl chloride is obtained in a yield of 74%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07977494B2 |
| Source dataset | uspto-grants-2011_07 |
| ORD ID | ord-ff3d0cfa89bf43d38cc4324d77036c5a |
| Source note | uspto-grants-2011_07 |