Water → 4-(5-Chloro-6-fluoropyridin-2-yl)morpholine
Reaktionsgleichung
[Cl:1]C1CC(=O)NC1=O.[F:9][C:10]1[N:15]=[C:14]([N:16]2[CH2:21][CH2:20][O:19][CH2:18][CH2:17]2)[CH:13]=[CH:12][CH:11]=1.O.C(Cl)Cl>C(#N)C>[Cl:1][C:11]1[CH:12]=[CH:13][C:14]([N:16]2[CH2:21][CH2:20][O:19][CH2:18][CH2:17]2)=[N:15][C:10]=1[F:9]Komponenten
6
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 70 °C
Versuchsvorschrift
Chlorosuccinimide (10.29 g, 77 mmol) was added to a solution of 4-(6-fluoropyridin-2-yl)morpholine (11.7 g, 64.2 mmol) in ACN (15 mL). The reaction mixture was heated to 70° C. for 30 min. Water and DCM were added. The organic phase was separated, washed with aqueous NaHCO3, brine and subsequently dried over MgSO4. The solvent was removed under reduced pressure and the residue was purified by silica gel chromatography (5-20% EtOAc/hexanes) to afford 3.11 g of 4-(5-chloro-6-fluoropyridin-2-yl)morpholine.
Aufarbeitung
- customThe organic phase was separated
- washwashed with aqueous NaHCO3, brine
- dry with materialsubsequently dried over MgSO4
- customThe solvent was removed under reduced pressure
- customthe residue was purified by silica gel chromatography (5-20% EtOAc/hexanes)
Quellen und Nachweise
- ORD-Eintrag
- ord-4b95d1f3a392427abf1063140f1479ca
- Quelldatensatz
- uspto-grants-2013_07
- Patentnummer
- US08497264B2
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