Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 3-Hydroxypyridine | HCID 7971 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | tert-Butyl (6-bromohexyl)carbamate | HCID 16211353 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 68677158 | HCID 68677158 | — |
Reaction Steps
3-Hydroxypyridine (262 mg) was added to a suspension of 60% sodium hydride (128 mg) in N,N-dimethylformamide (5 ml) and the mixture was stirred at 60° C. for 30 minutes. After cooling in ice a solution of N-(tert-butoxycarbonyl)-6-bromo-hexylamine (770 mg) (Helv. Chim. Acta 76 891 (1993) in N,N-dimethylformamide (3 ml) was added dropwise and stirring was continued overnight at room temperature. Ice and water were added and the mixture was extracted three times with diethyl ether. The organic phases were washed with saturated sodium chloride, dried and evaporated to leave a yellow oil which after purification by chromatography on silica gel with diethyl ether as eluent gave the desired compound as a colourless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07304066B2 |
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| Source dataset | uspto-grants-2007_12 |
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| ORD ID | ord-22299cfaccf744fea4df5922e040d4a7 |
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| Source note | uspto-grants-2007_12 |
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