Reaktion #41941

Reaktionsgleichung

4-Chloro-6-iodo-3-methanesulfonyl-2-methyl-quinoline

4-hydroxypiperidine

N,N-diisopropyl ethyl amine

→

white crystals

Ausbeute 62.1%

1-(6-Iodo-3-methanesulfonyl-2-methyl-quinolin-4-yl)-piperidin-4-ol

Ausbeute 62.1%

Lösungsmittel

N,N-dimethylformamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeN,N-Dimethylformamide was evaporated at 40° C./0.1 mbar
2. 2
   Sonstigethe residue directly purified by chromatography on silica gel in dichloromethane/methanol 20:1
3. 3
   SonstigeOne obtained a yellow oil which
4. 4
   Sonstigewas triturated with ethyl acetate
5. 5
   Filtrationthe resulting white crystals were filtered off

Vorschrift

4-Chloro-6-iodo-3-methanesulfonyl-2-methyl-quinoline (compound of example D.2) (300 mg, 0.786 mmol), 4-hydroxypiperidine (87 mg, 0.865 mmol) and N,N-diisopropyl ethyl amine (0.148 mL, 0.865 mmol) were heated in dry N,N-dimethylformamide (3 mL) for 0.5 h at 100° C. N,N-Dimethylformamide was evaporated at 40° C./0.1 mbar, and the residue directly purified by chromatography on silica gel in dichloromethane/methanol 20:1. One obtained a yellow oil which was triturated with ethyl acetate and the resulting white crystals were filtered off. One obtained 218 mg (62%) of white crystals. MS: m/z=447 (M+H).

Quelle