HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Aminopyridine → HCID 54717104, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Aminopyridine | HCID 10439 | — |
| Reactant | HCID 54717101 | HCID 54717101 | — |
| Solvent | O-Xylene | HCID 7237 | — |
| Product | HCID 54717104 | HCID 54717104 | — |
Reaction Steps
A mixture of 2.2 g. of 3-carbomethoxy-7-chloro-4-hydroxy-2-methyl-2H-thieno-[3,4-e]-1,2-thiazine-1,1-dioxide, 0.9 g. of 2-aminopyridine and 240 ml. of absolute o-xylene is boiled under reflux for 7 hours while stirring, approximately 80 ml. of the o-xylene being slowly distilled during the first 2 hours. After the reaction mixture has been cooled to room temperature, it is concentrated to approximately 60 ml. by evaporation in vacuo and cooled in an ice bath. The product that crystallizes out is suction filtered, washed with ether, dried and recrystallized from acetonitrile, and 7-chloro-4-hydroxy-2-methyl-3-(2-pyridylcarbamoyl)-2H-thieno[3,4-e]-1,2-thiazine-1,1-dioxide having a melting point of 218°-220° (with decomposition) is obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04180662 |
| Source dataset | uspto-grants-1979_12 |
| ORD ID | ord-ee0e02271bc7428e89be125b21e300aa |
| Source note | uspto-grants-1979_12 |