Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Oxalic Acid | HCID 971 | — |
| Reactant | Oxalate | HCID 71081 | — |
| Reactant | HCID 23454842 | HCID 23454842 | — |
| Catalyst | HCID 178418390 | HCID 178418390 | — |
| Solvent | HCID 178418361 | HCID 178418361 | — |
| Product | HCID 13020610 | HCID 13020610 | 73.8% |
Reaction Steps
A mixture of 442 mg of α-[(α,α-dimethyl-4-methoxyphenethylamino)methyl]-2-benzyloxybenzylalcohol hydrochloride, 250 mg of 10% palladium-carbon and 25 ml of 95% aqueous ethanol is shaken at room temperature in hydrogen gas atmosphere under atmospheric pressure. After the uptake of hydrogen is completed, insoluble materials are removed by filtration. The filtrate is evaporated to remove the solvent. The residue (colorless oil) is alkalized with an aqueous ammonia solution, whereby 300 mg of a pale yellow oil are obtained. Said oil is converted into its oxalate by using 45 mg of oxalic acid, and the oxalate is recrystallized from 95% aqueous methanol. 243 mg of α-[(α,α-dimethyl-4-methoxyphenethylamino)methyl]-2-hydroxybenzylalcohol 1/2 oxalate are thereby obtained as colorless needles.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04276304 |
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| Source dataset | uspto-grants-1981_06 |
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| ORD ID | ord-b0a7efe5bda54ff08859fc9d8a3e95f8 |
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| Source note | uspto-grants-1981_06 |
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