Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | 2,5-Dimethoxytetrahydrofuran | HCID 79098 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | L-Aspartic acid, 1,4-dimethyl ester, hydrochloride (1:1) | HCID 2734892 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 89493860 | HCID 89493860 | 69% |
Reaction Steps
Acetic acid (2.5 ml) and sodium acetate (32.5 mmol, 2.6 g) were added to a solution of dimethyl L-aspartate hydrochloride (29.5 mmol, 5.830 g) in dichloromethane (60 ml) and water (30 ml). Tetrahydro-2,5-dimethoxyfuran (29.5 mmol, 3.8 ml) was added to the resulting mixture heated at 80° C. After 90 min. the solution was cooled and the acqueous layer was washed with DCM. The combined organic layers were washed with brine and then dried, filtered and evaporated. The crude residue was purified by chromatograpgy on silica gel (eluent:Hex/AcOEt:7/3) to give the wanted compound as a colorless viscous oil (4.3 g, 68% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09181258B2 |
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| Source dataset | uspto-grants-2015_11 |
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| ORD ID | ord-7f8c02f387da44d2ad86b20864fdd757 |
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| Source note | uspto-grants-2015_11 |
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