Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 178499754 | HCID 178499754 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 57899233 | HCID 57899233 | 27% |
| Product | HCID 57899291 | HCID 57899291 | 21% |
Reaction Steps
To a solution of (E)-3-(4-{1-[2-(1H-tetrazol-5-yl)-ethyl]-pyrrolidin-2-yl}-phenyl)-acrylic acid methyl ester (1.0 g, 2.1 mmol) in dimethylformamide (5 mL) was added iodomethane (1.91 mL, 30.6 mmol) and sodium hydroxide (1.64 g, 30.7 mmol). The reaction was stirred at room temperature for 2 h, ice water was added, and the resulting mixture was extracted several times with ethyl acetate. The combined organic layers were washed with a saturated aqueous solution of sodium chloride, dried over sodium sulfate, filtered and concentrated in vacuo. The residue was purified via silica gel column chromatography to give (E)-3-(4-{1-[2-(2-methyl-2H-tetrazol-5-yl)-ethyl]-pyrrolidin-2-yl}-phenyl)-acrylic acid methyl ester (0.15 g, 21%, LCMS (m/z): 342.1 (M+1)) and (E)-3-(4-{1-[2-(1-methyl-1H-tetrazol-5-yl)-ethyl]-pyrrolidin-2-yl}-phenyl)-acrylic acid methyl ester (0.20 g, 27%, LCMS (m/z): 342.1 (M+1)).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07943652B2 |
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| Source dataset | uspto-grants-2011_05 |
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| ORD ID | ord-d47ef658e76340f7bbd29b31ea9a6bf0 |
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| Source note | uspto-grants-2011_05 |
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