Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 18422339 | HCID 18422339 | — |
| Reactant | Potassium tert-butoxide | HCID 23665647 | — |
| Solvent | 1,2-Dimethoxyethane | HCID 8071 | — |
| Product | HCID 18422308 | HCID 18422308 | 35.2% |
Reaction Steps
Potassium tert-butoxide (718 mg) was suspended in 1,2-dimethoxyethane (35 ml) and the mixture was refluxed under heating. Thereto was added dropwise ethyl 2-(2-aminoanilino)benzo[b]thiophene-3-carboxylate (1.0 g) dissolved in 1,2-dimethoxyethane (35 ml) over 15 minutes. After 30 minutes, potassium tert-butoxide (359 mg) was added and the mixture was refluxed under heating for 1 hour. After the completion of the reaction, the reaction mixture was allowed to cool to room temperature and poured into 0.5N hydrochloric acid. The mixed solution was extracted 3 times with chloroform, and washed with water and dried over magnesium sulfate. The solution was filtered and the solvent was evaporated under reduced pressure. The precipitated crude crystals were washed with ethyl acetate and diisopropyl ether to give 6H-[1]benzothieno[2,3-b][1,5]benzodiazepin-12(11H)-one (300 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06455521B1 |
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| Source dataset | uspto-grants-2002_09 |
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| ORD ID | ord-42caf3ff6bab47e3a2e7cd965bbe34cb |
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| Source note | uspto-grants-2002_09 |
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