Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 89932943 | HCID 89932943 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 84653624 | HCID 84653624 | 87.3% |
Reaction Steps
To a mixture of 7-chloro-5-nitro-2,3-dihydro-1-benzofuran (7.40 g) and ethanol (300 mL) were added reduced iron (12.4 g) and concentrated hydrochloric acid (20.0 mL) under ice-cooling, followed by warming to room temperature and stirring overnight. This mixture was neutralized with a saturated aqueous sodium hydrogen carbonate solution and sodium hydrogen carbonate under ice-cooling, filtered through celite, and then extracted with ethyl acetate. The organic layer was washed with saturated brine and then dried over anhydrous sodium sulfate, the insoluble materials were separated by filtration, and the filtrate was concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate=80:20 to 60:40) to obtain 7-chloro-2,3-dihydro-1-benzofuran-5-amine (5.49 g) as a pale yellow solid.
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-bf1eead56ecd4b3a812aa018d5d21139 |
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| Source note | uspto-grants-2016_02 |
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