Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Fumaric Acid | HCID 444972 | — |
| Reactant | HCID 57168040 | HCID 57168040 | — |
| Solvent | Isopropanol | HCID 3776 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 67751258 | HCID 67751258 | 78% |
Reaction Steps
4.27 g of N-[2-((1R,3R,4S)-1-methyl-4-isopropylcyclohex-3-yloxy)ethyl]-N-[2-(3,4-dimethoxybenzyloxy)ethyl]-N-methylamine base were dissolved in 50 ml of tetrahydrofuran. A solution of 1.22 g of fumaric acid in 15 ml of isopropanol was added to the solution. The solution was concentrated to a volume of about 20 ml under reduced pressure, and a mixture of diethyl ether/n-hexane was added until the solution became cloudy, after which the solution was cooled to 0° C. The precipitated crystals were filtered out and dried at 50° C. 4.28 g of N-[2-((1R,3R,4S)-1-methyl-4-isopropylcyclohex-3-yloxy)et hyl]-N-[2-(3,4-dimethoxybenzyloxy)ethyl]-N-methylamine fumarate having a melting point of 72° C.-73° C. were obtained. [α]D20 =-37.0° (c=1; methanol)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05212173 |
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| Source dataset | uspto-grants-1993_05 |
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| ORD ID | ord-066fc7b4dd914816bff6bb8eadfbf488 |
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| Source note | uspto-grants-1993_05 |
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