HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Diisopropylethylamine → tert-Butyl 1-(2-(trifluoromethyl)pyridin-4-yl)piperidin-4-ylcarbamate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Diisopropylethylamine | HCID 81531 | — |
| Edukt | 4-Amino-1-Boc-piperidine | HCID 1268291 | — |
| Edukt | 4-Iodo-2-(trifluoromethyl)pyridine | HCID 23436940 | — |
| Lösungsmittel | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Produkt | tert-Butyl 1-(2-(trifluoromethyl)pyridin-4-yl)piperidin-4-ylcarbamate | HCID 67342449 | 76,4% |
Reaktionsschritte
To a mixture of 4-iodo-2-(trifluoromethyl)pyridine (356 mg, 1.3 mmol) and Boc-4-aminopiperidine (340 mg, 1.7 mmol) in NMP (2.6 mL) was added DIPEA (319 L, 1.83 mmol). Argon was bubbled through the cloudy solution for 5 minutes before the reaction mixture was heated in the microwave for 3×30 minutes to 150° C. The mixture was then poured into water and extracted with ethyl acetate. The combined organic phases were dried over sodium sulfate, filtered and evaporated. Purification by chromatography (silica gel, 50 g, 0 to 100% ethyl acetate in heptane) afforded the title compound (343 mg, 76%) as a white solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08486967B2 |
| Quelldatensatz | uspto-grants-2013_07 |
| ORD ID | ord-97a5cba06aba46a4b17d85304e4b67f4 |
| Quellennotiz | uspto-grants-2013_07 |