Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Toluene | HCID 1140 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Red-Al | HCID 16684438 | — |
| Reactant | HCID 68810951 | HCID 68810951 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 68813248 | HCID 68813248 | — |
Reaction Steps
To a mixture of (2R,3S)-8-methyl-3-(2-thienyl)-8-aza-bicyclo[3.2.1]octane-2-carboxylic acid ethyl ester (3.65 g, 13.75 mmol) and toluene (75 ml), Red-Al (6 ml, 65%, 20 mmol) was added at 0° C. The mixture was stirred at 0° C. for 1 h. A solution of aqueous sodium hydroxide (20 ml, 4 M) was added dropwise followed by warm water (50° C., 150 ml). The mixture was extracted with toluene (2×100 ml). The mixture was dried (MgSO4) and evaporated. The product was isolated as crystals. Mp: 153.7-157.5° C. Yield 2.04 g (63%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07247643B2 |
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| Source dataset | uspto-grants-2007_07 |
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| ORD ID | ord-d89c7d615e5247309213fca1dd7ad8f4 |
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| Source note | uspto-grants-2007_07 |
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