HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ethanol → 4-amino-4-methyl-N-(2-pyrimidinyl)piperidine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ethanol | HCID 702 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | 2-Chloropyrimidine | HCID 74404 | — |
| Edukt | 4-Methylpiperidin-4-amine | HCID 21090445 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 4-amino-4-methyl-N-(2-pyrimidinyl)piperidine | HCID 21882566 | 65,1% |
Reaktionsschritte
2 ml of an ethanol suspension containing 260 mg of 4-amino-4-methylpiperidine (synthesized according to a method described in U.S. Pat. No. 5,821,240), 237 mg of 2-chloropyrimidine and 858 mg of potassium carbonate was stirred at 50° C. for 12 hours. The reaction mixture was poured into water, and extracted with chloroform. The extract was washed with brine, dried over anhydrous sodium sulfate, and the solvent was removed under reduced pressure. The residue was purified by silica gel flash column chromatography [solvent: chloroform-methanol-aqueous ammonia (300:10:1)] to obtain 259 mg of 4-amino-4-methyl-N-(2-pyrimidinyl)piperidine (Reference Example 8-1 in Table 9).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07138397B2 |
| Quelldatensatz | uspto-grants-2006_11 |
| ORD ID | ord-053d787a165944de89f3ae46539e47f4 |
| Quellennotiz | uspto-grants-2006_11 |