Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Diethylamine | HCID 8021 | — |
| Edukt | 2-Chloronicotinoyl chloride | HCID 2774541 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 2-Chloro-N,N-diethylnicotinamide | HCID 4465944 | — |
Reaktionsschritte
Into a 1-neck round-bottom flask under an atmosphere of nitrogen was dissolved 2-chloronicotinoyl chloride (2.12 g, 0.0120 mol) in methylene chloride (25 mL) and the reaction cooled to 0° C. N-ethylethanamine (2.7 mL, 0.026 mol) was added to the mixture and stirred at 0° C. for 2 hours and then at 20° C. for 16 hours. The reaction was extracted with dichloromethane and the organic extracts were washed with water, brine, dried (MgSO4), and concentrated in vacuo. The crude product was used in the next reaction without further purification. 1H NMR (400 MHz, CDCl3): δ 8.42-8.44 (m, 1H), 7.64-7.65 (m, 1H), 7.29-7.63 (m, 1H), 3.75-3.79 (m, 1H), 3.35-3.40 (m, 1H), 3.13-3.22 (m, 2H), 1.82 (t, 3H), 1.088 (t, 3H). MS: [M+1]=213.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08835423B2 |
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| Quelldatensatz | uspto-grants-2014_09 |
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| ORD ID | ord-088b137e3b034d10b39a478428906864 |
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| Quellennotiz | uspto-grants-2014_09 |
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