HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 22393132, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | HCID 22393105 | HCID 22393105 | — |
| Solvent | Oxolane--water (1/1) | HCID 21881883 | — |
| Product | HCID 22393132 | HCID 22393132 | 96.3% |
Reaction Steps
Lithium hydroxide (0.062 g) was added to a solution of 1,1-dioxo-3,3-dibutyl-5-phenyl-7-methoxy-8-ethoxycarbonylmethoxy-2,3,4,5-tetrahydro-1,5-benzothiazepine (Method 45; 0.448 g, 0.865 mmol) in THF/H2O (2/1, 6 ml). After 1 hour AcOH (0.5 ml) was added and most of the solvent was removed under reduced pressure. The crude product was purified by HPLC (MeCN) to give the title compound 0.408 g (96%) as a white solid. NMR (400 MHz, CD3OD): 0.75-0.85 (m, 6H), 1.00-1.30 (m, 8H), 1.35-1.55 (m, 4H), 3.20 (s, 2H), 3.65 (s, 3H), 3.70 (brs, 2H), 4.50 (s, 2H), 6.50 (s, 1H), 6.90-7.30 (m, 5H),
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06906058B2 |
| Source dataset | uspto-grants-2005_06 |
| ORD ID | ord-2670f0c6313347eb9ac670a2c401eff5 |
| Source note | uspto-grants-2005_06 |