Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Sodium methanethiolate | HCID 4378561 | — |
| Reactant | HCID 22393109 | HCID 22393109 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 18442440 | HCID 18442440 | 96% |
Reaction Steps
1,1-Dioxo-3,3-dibutyl-5-phenyl-7-bromo-8-carboxymethoxy-2,3,4,5-tetrahydro-1,5-benzothiazepine (Method 14; 500 mg, 0.93 mmol) was dissolved in DMF (10 ml). Sodium methanethiolate (200 mg, 2.85 mmol) was added and the mixture was stirred for 2 hours at 50° C. Acetic acid (0.4 ml) was added and the solvent was evaporated under reduced pressure. The residue was extracted with EtOAc/water. The EtOAc layer was separated, dried and evaporated under reduced pressure to give, the title compound 450 mg (96%). NMR. (300 MHz) 0.7–0.8 (m, 6H), 1.0–1.6 (m, 12H), 2.2 (s, 2H), 3.2 (brs, 2H), 3.7 (brs, 2H), 4.8 (s, 2H), 6.6 (s, 1H), 6.9–7.1 (m, 3H), 7.2–7.4 (m, 3H).
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-614d687bece14db68704b2c7d2a21556 |
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| Source note | uspto-grants-2007_03 |
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