Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Chloride | HCID 5234 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | HCID 15587270 | HCID 15587270 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 135430559 | HCID 135430559 | 64.7% |
Reaction Steps
A mixture of 0.44 g of 1-(4-methoxy-3-acetoxyphenyl)-4-methyl-5-ethyl-7-acetoxy-8-methoxy-5H-2,3-benzodiazepine, 8 ml of ethanol, 8 ml of water and 0.4 g of potassium hydroxide is stirred in nitrogen atmosphere for 15 minutes. 50 ml of 20% aqueous sodium chloride solution and 0.6 g of ammonium chloride are added to the solution. The precipitate is separated and recrystallized from 7.5 ml of 20% aqueous dimethyl formamide. 0.23 g of pure 1-(4-methoxy-3-hydroxyphenyl)-4-methyl-5-ethyl-7-hydroxy-8-methoxy-5H-2,3-benzodiazepine are obtained; the product decomposes at 210°-212° C. This compound is identical with the product obtained according to Example 26, and no depression of melting point can be observed when admixing the two products with each other.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04322346 |
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| Source dataset | uspto-grants-1982_03 |
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| ORD ID | ord-e9d4a2a6d120456cb0c28c5e2bf61470 |
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| Source note | uspto-grants-1982_03 |
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