HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 13922885, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Dimethylcarbamoyl Chloride | HCID 6598 | — |
| Reactant | HCID 13922842 | HCID 13922842 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 13922885 | HCID 13922885 | 75% |
Reaction Steps
A solution of 2.3 g (10 mmoles) of 5-hydroxy-2-sulfamoylbenzo[b]thiophene in 50 ml of pyridine was treated with 200 mg of 4-dimethylaminopyridine and finally 2.5 ml (2.9 g, 27 mmoles) of dimethylcarbamyl chloride. The resultant clear solution was stirred at room temperature for 48 hours, when it was poured into a mixture of 200 g of chopped ice and 100 ml of concentrated HCl. The precipitated solid was collected and washed with cold H2O until the washings were neutral. Drying gave 2.25 g (75%) of tan powder which was crystallized from isopropyl alcohol to give 1.6 g of product, m.p. 192°-194° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04668697 |
| Source dataset | uspto-grants-1987_05 |
| ORD ID | ord-7d01d68313f64a419d904c71e87980c8 |
| Source note | uspto-grants-1987_05 |