Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Chloroform | HCID 6212 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 13175689 | HCID 13175689 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 13175690 | HCID 13175690 | — |
Reaction Steps
A solution of 11 g of 7-chloro-1-(β-chloroethyl)-2-chloromethyl-5-(3-thienyl)-2,3-dihydro-1H-1,4-benzodiazepine in 60 ml of dioxane and 160 ml of 4.5% strength sodium hydroxide solution is heated under reflux for 5 hours. After the solvent has been stripped off in vacuo, the reaction product is isolated from chloroform and is then chromatographed on aluminum oxide of activity level II, using methylene chloride. After the methylene chloride has been stripped off, 6.5 g of 1,2,4,4a-tetrahydro-9-chloro-7-(3-thienyl)-5H-[1,4]oxazino[4,3-a][1,4]benzodiazepine are obtained as an oil. This product is converted into its hydrochloride by reaction with alcoholic hydrogen chloride solution, and the product is crystallised as the hydrochloride.0.3H2O from isopropanol. Melting point: 207° to 212° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04594436 |
|---|
| Source dataset | uspto-grants-1986_06 |
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| ORD ID | ord-0c3cc1e3a1934b41ad6f2eacfaa0d817 |
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| Source note | uspto-grants-1986_06 |
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