Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | HCID 23362616 | HCID 23362616 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 15919157 | HCID 15919157 | 111.5% |
Reaction Steps
Six (6) g of hydrogenation catalyst in which 5 % of Pd was carried on activated carbon and a small amount of sodium acetate were placed in an eggplant-shaped flask. After replacing the atmosphere inside the flask with nitrogen, 6 g of the above Compound D dissolved in 90 ml of dioxane was slowly dropped into the flask through a dropping funnel. After replacing the inside atmosphere with hydrogen with stirring, hydrogen was supplied from a gas reservoir. The reaction was continued until hydrogen absorption ceased. Thereafter the atmosphere was replaced with nitrogen, and the catalyst was removed by filtration. The solvent was recovered from the filtrate. Thus obtained crude product was purified by column chromatography and recrystallization to provide 6.1 g of purified 2-(4-octyloxyphenyl)-5- ethoxycarbonylpyrimidine (Compound E).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05587106 |
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| Source dataset | uspto-grants-1996_12 |
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| ORD ID | ord-e69a65ee5681407a87c3a61141e4b526 |
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| Source note | uspto-grants-1996_12 |
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