Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | n-(5-Tert-butylthiazol-2-yl)-5-chloro-2-methoxybenzamide | HCID 87094486 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | HCID 178490667 | HCID 178490667 | — |
Reaktionsschritte
A solution of Example 244A (75 mg, 0.23 mmol) in N,N-dimethylformamide (2 mL) was treated with NaH 60% dispersion in oil (9.5 mg, 0.23 mmol) followed by Example 308A (60 mg, 0.23 mmol). The reaction mixture was stirred at room temperature for 18 hours, poured into water and extracted with ethyl acetate. The organic layer was washed with H2O (2×50 mL), dried over MgSO4, filtered, concentrated under reduced pressure and dried under vacuum (˜1 mm Hg) to afford the title compound. 1H NMR (300 MHz, dimethylsulfoxide-d6) δ ppm 1.17 (s, 6H), 1.32 (s, 9H), 1.76-1.91 (m, 2H), 3.79 (s, 3H), 4.14-4.31 (m, 2H), 4.43 (s, 1H), 7.10 (d, J=8.8 Hz, 1H), 7.31 (s, 1H), 7.44 (dd, J=9.0, 2.9 Hz, 1H), 7.76 (d, J=3.1 Hz, 1H); MS (ESI) m/z 411 (M+H)h Anal. Calculated for C20H27ClN2O3SC, 58.45; H, 6.62; N, 6.82. Found C, 58.30; H, 6.51; N, 6.71.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08841334B2 |
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| Quelldatensatz | uspto-grants-2014_09 |
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| ORD ID | ord-57ab2a46a4b348289f06e63ff1584e1a |
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| Quellennotiz | uspto-grants-2014_09 |
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