Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | 1-Butanol | HCID 263 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 10949234 | HCID 10949234 | — |
| Solvent | 1,2-Dimethoxyethane | HCID 8071 | — |
| Product | HCID 21199124 | HCID 21199124 | — |
Reaction Steps
A mixture of n-butanol (5 ml) and sodium hydride (60% in oil, 20 mmol) is stirred until the formation of H2 gas ceases. A mixture of 1C (2.0 g, 5.0 mmol) and dimethoxyethane (15 ml) is added to the resulting reaction mixture. Subsequently, the reaction mixture is heated to 90° C. with stirring for 14 hours and dimethoxyethane is distilled off. A mixture of water and ethyl acetate (1:1 v/v; 100 ml) is then slowly added at room temperature. The organic phase is separated, concentrated and the residue is purified by column chromatography (petrol ether: ethyl acetate, 90:10 v/v) yielding the pure product as a yellow oil, 1.7 g (78.3%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US06242498B1 |
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| Source dataset | uspto-grants-2001_06 |
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| ORD ID | ord-b927853de59045fcb36cbb6497d500ce |
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| Source note | uspto-grants-2001_06 |
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