HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 3715801, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | HCID 20092951 | HCID 20092951 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 3715801 | HCID 3715801 | — |
Reaction Steps
To ice-cooled DMF (4.0 g) was added phosphorous oxychloride (8.4 g) dropwise and the mixture was stirred at room temperature for 15 minutes. To the stirred reaction mixture was added a solution of 1-(2-chloro-4-methylphenyl)pyrrole (9.7 g) in DMF (8 ml) dropwise and the mixture was stirred at 50° C. for 1.5 hours followed by addition of ice-water. Stirring was continued for a while and then the mixture was made basic with potassium carbonate, and extracted with ethyl acetate. The extract was washed with water, dried and evaporated. The residue was purified by column chromatography on silica gel to give crystals. Recrystallization from ethyl acetate-hexane afforded yellow prisms (7.1 g, 59%), m.p. 111°-112° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05389641 |
| Source dataset | uspto-grants-1995_02 |
| ORD ID | ord-b7aded1f56ba489695316f944428d229 |
| Source note | uspto-grants-1995_02 |