HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Potassium Carbonate → N-[2-[4-(6-Fluoro-1,2-benzisoxazol-3-yl)-1-piperidinyl]ethyl]morpholine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | Morpholine, 4-(2-chloroethyl)-, hydrochloride (1:1) | HCID 77210 | — |
| Edukt | 3-(4-Piperidyl)-6-fluoro-1,2-benzisoxazole | HCID 849421 | — |
| Lösungsmittel | Acetonitrile | HCID 6342 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | N-[2-[4-(6-Fluoro-1,2-benzisoxazol-3-yl)-1-piperidinyl]ethyl]morpholine | HCID 21960100 | — |
Reaktionsschritte
A mixture of 6-fluoro-3-(4-piperidinyl)-1,2-benzisoxazole (3.0 g, 13.6 mmol), 2-chloroethyl morpholine hydrochloride (4.46 g, 29.7 mmol) and K2CO3 (7.3 g, 2.2 eq) in acetonitrile (60 ml) was heated at reflux for 24 hours. The crude mixture was diluted with DCM and filtered. The solvent was concentrated to an oil (~7.1 g). Purification on a silica gel column (55 g, SiO2, eluted with MeOH:DCM) yielded a solid product weighing 4 g. Recrystallization from hot ethanol yielded 2.1 g (48%), m.p.=131°-132° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05591745 |
| Quelldatensatz | uspto-grants-1997_01 |
| ORD ID | ord-664ff15ce0564cbb8f3b235bae14be18 |
| Quellennotiz | uspto-grants-1997_01 |