Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | D-Tartaric acid | HCID 439655 | — |
| Reactant | HCID 45380480 | HCID 45380480 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 86640697 | HCID 86640697 | — |
Reaction Steps
The salt was prepared by dissolving the starting material from Example 164C (275. mg, 0.775 mmol) in ethyl acetate (5.0 mL) and ethanol (1.0 mL) then adding (2S,3S)-2,3-dihydroxysuccinic acid (128 mg, 0.852 mmol, dissolved in a minimal amount of methanol) slowly and stirring rapidly over night. The material precipitated to give a white solid. The solid was collected by filtration and dried under vacuum to give the titled compound: 1H NMR (300 MHz, methanol-d4) δ ppm 1.97-2.13 (m, 2H) 2.19-2.37 (m, 2H) 3.38-3.51 (m, 3H) 3.51-3.69 (m, 2H) 4.41 (s, 2H) 4.70 (s, 2H) 5.54 (s, 2H) 6.89-7.05 (m, 1H) 7.18 (dd, J=9.32, 2.58 Hz, 1H) 7.32-7.50 (m, 3H) 8.05 (s, 1H); MS (DCI/NH3) m/z 356 (M+H)+. Anal. Calcd. for C20H19ClFN3.C4H6O6: C, 56.98; H, 4.97; 8.31. Found: C, 56.71; H, 4.88; N, 8.20.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09063126B2 |
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| Source dataset | uspto-grants-2015_06 |
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| ORD ID | ord-6817c690223540aaab2d42f04eb7edc1 |
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| Source note | uspto-grants-2015_06 |
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