Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | tert-Butanol | HCID 6386 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | P,P-Diphenylphosphinic azide | HCID 199401 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 2,3-Dihydrobenzo(b)furan-5-carboxylic acid | HCID 676583 | — |
| Product | HCID 65143109 | HCID 65143109 | — |
Reaction Steps
To a mixture of 2,3-dihydro-1-benzofuran-5-carboxylic acid (5.08 g), triethylamine (5.18 mL) and tert-butanol (91.9 mL) was added diphenylphosphoryl azide (8.00 mL), followed by stirring at 90° C. for 5 hours. The reaction mixture was poured into a saturated aqueous sodium hydrogen carbonate solution, followed by extraction with ethyl acetate. The organic layer was washed with a saturated aqueous sodium hydrogen carbonate solution and saturated brine, and dried over anhydrous sodium sulfate. The insoluble materials were separated by filtration, the filtrate was concentrated under reduced pressure, and the obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate=20:1 to 5:1) to obtain tert-butyl (2,3-dihydro-1-benzofuran-5-yl)carbamate (4.74 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09260445B2 |
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| Source dataset | uspto-grants-2016_02 |
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| ORD ID | ord-a47a070c83494252ba13cf934e5d9423 |
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| Source note | uspto-grants-2016_02 |
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