Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 53897782 | HCID 53897782 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 18315358 | HCID 18315358 | 109.9% |
Reaction Steps
A 1N aqueous solution of sodium hydroxide (1.5 ml) was added to a methanol solution (6 m.) of 5-(3-tert-butyloxycarbonylaminomethylphenyl)-7-chloro-2,3-dihydro-2-oxo-1H-1,4-benzodiazepine-3-acetic acid methyl ester (0.6 g), the compound produced in Example 97-(1). The mixture was stirred for 2 hours at 60° C. The reaction mixture was diluted with water (50 ml), which was acidified, followed by extraction with ethyl acetate (50 ml) twice. The extracts were combined and washed with a saturated aqueous saline solution, followed by drying over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to give 5-(3-tert-butyloxycarbonylaminomethylphenyl)-7-chloro-2,3-dihydro-2-oxo-1H-1,4-benzodiazepine-3-acetic acid (0.64 g) as a colorless amorphous solid product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06352982B1 |
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| Source dataset | uspto-grants-2002_03 |
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| ORD ID | ord-2e1561014b434e7b8fe0ad2716f4f798 |
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| Source note | uspto-grants-2002_03 |
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