Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 53982694 | HCID 53982694 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 22903450 | HCID 22903450 | 92.4% |
Reaction Steps
In ethanol (8 ml) was dissolved (3RS,5SR,αSR)-7-chloro-5-(2-chlorophenyl)-1-isopropyl-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-glycolic acid ethyl ester (0.3 g) obtained in Example 1. To the solution was added 1N sodium hydroxide (2 ml), and the mixture was left standing for 20 minutes at room temperature. To the resultant mixture was added 1N hydrochloric acid (50 ml) to make the solution acid, followed by extraction with ethyl acetate (50 ml). The extract solution was washed with water, dried over anhydrous magnesium sulfate, then the solvent was distilled off under reduced pressure to give (3RS,5SR,αSR)-7-chloro-5-(2-chlorophenyl)-1-isopropyl-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-glycolic acid (0.26 g) as prisms, m.p. 245°-247° C. (decomp.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05677298 |
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| Source dataset | uspto-grants-1997_10 |
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| ORD ID | ord-1ab2e4f6cb5a4e6b9f5b956d9c33c928 |
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| Source note | uspto-grants-1997_10 |
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