Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 22393120 | HCID 22393120 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 22393108 | HCID 22393108 | 97.2% |
Reaction Steps
1,1-Dioxo-3-butyl-3-ethyl-5-phenyl-7-methoxy-8-ethoxycarbonylmethoxy-2,3,4,5-tetrahydro-1,5-benzothiazepine (Method 7; 1.2 g) was dissolved in ethanol (20 ml). Sodium hydroxide (0.5) dissolved in H2O (1 ml) was added and the reaction mixture was warmed to 40° C. for 30 min. Acetic acid (1 ml) was added and the solvent was removed at reduced pressure. The residue was partitioned between DCM/H2O and the organic layer was separated and dried. Trituration of the residue with n-hexane gave the title compound 1.1 g (97%) as a solid. NMR 0.75–0.85 (m, 3H), 0.9 (t, 3H), 1.0–1.7 (m, 8H), 3.2 (q, 2H), 3.65 (s, 3H), 3.65–3.85 (m, 2H), 4.7 (s, 2H), 6.4 (s, 1H), 7.0 (t, 1H), 7.1 (d, 2H), 7.3 (t, 2H), 7.5 (s, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07192945B2 |
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| Source dataset | uspto-grants-2007_03 |
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| ORD ID | ord-841c3335052245dca3c850cd698643fa |
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| Source note | uspto-grants-2007_03 |
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