HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → HCID 18442469, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 22393126 | HCID 22393126 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 18442469 | HCID 18442469 | 79.2% |
Reaction Steps
1,1-Dioxo-3-butyl-3-ethyl-5-phenyl-7-(ethoxycarbonylmethoxy)-2,3,4,5-tetrahydro-1,5-benzothiazepine (Method 3; 110 mg, 0.24 mmol) and sodium hydroxide (100 mg, 2.5 mmol) were added to ethanol (5 ml, 95%). The mixture was refluxed for 1 h. AcOH (0.30 ml) was added and the reaction mixture was evaporated under reduced pressure. The residue was extracted with DCM/water. The DCM layer was separated, dried and evaporated under reduced pressure. The residue crystallised when treated with hexane. 82 mg (79%) of the title compound was obtained. NMR (500 MHz): 0.7-0.9 (m, 6H), 1.1-1.7 (m, 8H), 3.1-3.25 (m, 2H), 3.6-3.8 (br d, 2H), 4.6 (s, 2H), 6.9-7.1 (m, 5H), 7.2-7.3 (m, 2H),
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06906058B2 |
| Source dataset | uspto-grants-2005_06 |
| ORD ID | ord-b9b4f19892ad4634a1dea07dc58322a7 |
| Source note | uspto-grants-2005_06 |