Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Diisopropylethylamine | HCID 81531 | — |
| Edukt | 3-Chloro-2-fluoro-5-(trifluoromethyl)pyridine | HCID 1268075 | — |
| Edukt | (S)-pyrrolidine-2-carboxylic acid (4-tert-butyl-thiazol-2-yl)-amide | HCID 54959952 | — |
| Lösungsmittel | Dimethyl Sulfoxide | HCID 679 | — |
| Produkt | HCID 86666036 | HCID 86666036 | — |
Reaktionsschritte
To a vial containing (S)-pyrrolidine-2-carboxylic acid (4-tert-butyl-thiazol-2-yl)-amide; hydrochloride (0.212 g; 0.731 mmol) in dimethylsulfoxide (2 mL) is added N,N-diisopropylethylamine (0.127 mL; 0.731 mmol) and 3-chloro-2-fluoro-5-trifluoromethylpyridine (0.096 mL; 0.731 mmol). The mixture is heated at 100° C. for 1 hour in an oil bath and then cooled to room temperature. The crude mixture is filtered and purified by preparative HPLC chromatography. Product fractions are pooled and concentrated in vacuo to afford title compound. ESI m/z 433 [M+H]+
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08629157B2 |
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| Quelldatensatz | uspto-grants-2014_01 |
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| ORD ID | ord-8bcb9c11fc4f4614bdb451cb936af102 |
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| Quellennotiz | uspto-grants-2014_01 |
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