Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Lithium borohydride | HCID 4148881 | — |
| Reactant | HCID 10623819 | HCID 10623819 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 10811188 | HCID 10811188 | 80.4% |
Reaction Steps
To a suspension of 1-(2-bromo-6-pyridyl)-2,3-bis(methoxycarbonyl)-6,7-dimethoxynaphthalene (715 mg) in tetrahydrofuran (20 ml) is added lithium borohydride (174 mg), and the mixture is refluxed. To the mixture is added dropwise a mixture of methanol (2.2 ml) and tetrahydrofuran (10 ml) under reflux over a period of two hours. After the reaction is complete, the mixture is concentrated under reduced pressure to remove the solvent, and ethyl acetate and water are added to the residue. The ethyl acetate layer is separated, washed, dried, and concentrated under reduced pressure to remove the solvent. The residue is purified by silica gel column chromatography (solvent; chloroform:methanol=15:1) to give 1-(2-bromo-6-pyridyl)-2,3-bis(hydroxymethyl)-6,7-dimethoxynaphthalene (505 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06005106 |
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| Source dataset | uspto-grants-1999_12 |
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| ORD ID | ord-c4cdbae2917f4f24947e1615cff5ea31 |
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| Source note | uspto-grants-1999_12 |
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