Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Fumaric Acid | HCID 444972 | — |
| Reactant | HCID 69829475 | HCID 69829475 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 22715133 | HCID 22715133 | 49% |
Reaction Steps
The product from step (a) (0.20 g, 0.42 mmol) was dissolved in 4M hydrogen chloride in dioxan (10 ml) and stirred for 3hat room temperature. The solvent was evaporated and the residue partitioned between ethyl acetate (50 ml) and aqueous saturated sodium bicarbonate solution (50 ml). The layers were separated and the aqueous portion was extracted with ethyl acetate (2×50 ml). The combined organic portions were washed with water (3×30 ml), dried (magnesium sulphate) and evaporated. The residue was dissolved in methanol and treated with one equivalent of fumaric acid, stirred for ten minutes and then the solvent was removed in vacuo. The solid residue was triturated with ethyl acetate and the white solid obtained filtered off and dried to give the title compound (0.10 g, 49%).,
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06743939B2 |
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| Source dataset | uspto-grants-2004_06 |
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| ORD ID | ord-a3c7dc4c66cb4f80bb6b4abed17a1654 |
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| Source note | uspto-grants-2004_06 |
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