Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Fumaric Acid | HCID 444972 | — |
| Reactant | HCID 9874451 | HCID 9874451 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 9874450 | HCID 9874450 | 88.3% |
Reaction Steps
To a solution of (S)-(−)-2-(3,5-di-tert-butyl-4-hydroxyphenyl)-3-[3-[N-methyl-N-[2-(3,4-methylenedioxy-phenoxy)ethyl]amino]propyl]-1,3-thiazolidin-4-one (569 mg, 1.05 mmol) in ethyl acetate (2 ml) was added a solution of fumaric acid (116 mg, 1.00 mmol) in methanol (3 ml) (prepared under preheating) and the mixture was stirred, then the solvent was removed under reduced pressure. The residue was dissolved in ethyl acetate (1 ml) under heating and the mixture was stirred at room temperature for 15 hours. The precipitate was filtered off, washed with ethyl acetate:n-hexane (1:1) and dried to give white crystals (582 mg). mp: 142-144° C.; Elementary analysis: calculated for C34H46N2O9: C, 61.99, H, 7.04, N, 4.25; found: C, 61.77, H, 7.09, N, 4.07.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06191281B1 |
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| Source dataset | uspto-grants-2001_02 |
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| ORD ID | ord-539626794cb94a8081219ca2e25a348e |
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| Source note | uspto-grants-2001_02 |
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