HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 10923302, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | HCID 10914818 | HCID 10914818 | — |
| Reactant | Sodium Methoxide | HCID 10942334 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 10923302 | HCID 10923302 | 106.5% |
Reaction Steps
A solution of N-(2-hydroxy-3-methoxyphenyl)-2-bromo-5-methyl-3-thiophenecarboxamide (2.30 g) and sodium methoxide (549 mg) in N,N-dimethylformamide (12 ml) was stirred under reflux with heating for 19 hours. The reaction system was cooled to room temperature, and the reaction mixture was poured into water (50 ml). The mixture was neutralized with hydrochloric acid, extracted twice with chloroform and washed with water. The organic layer was dried over sodium sulfate and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (elution solvent hexane:ethyl acetate=1:1) to give 2-methyl-9-methoxythieno[2,3-b][1,5]benzoxazepin-4(5H)-one (1.87 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06271225B1 |
| Source dataset | uspto-grants-2001_08 |
| ORD ID | ord-50ea0d7b1f314f55a80a0d7bb47d4ad9 |
| Source note | uspto-grants-2001_08 |