Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 59239861 | HCID 59239861 | — |
| Product | HCID 59239858 | HCID 59239858 | — |
Reaction Steps
tert-Butyl 1-[4-(ethoxycarbonyl)phenyl]hydrazinecarboxylate (5.60 g) and acetic anhydride (10 ml) were mixed, and the mixture was stirred at 90° C. for 1 hr. The reaction mixture was neutralized with 1N aqueous sodium hydroxide solution, and washed with water and saturated brine. The organic layer was dried over sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=19:1 (volume ratio)→1:1 (volume ratio)), and further recrystallized from ethyl acetate-hexane to give the title compound (4.42 g) as colorless crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07989445B2 |
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| Source dataset | uspto-grants-2011_08 |
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| ORD ID | ord-0be8f64e73cb4e06a62096cdb94d78e8 |
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| Source note | uspto-grants-2011_08 |
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