Reaktionsgleichung
Cl.[CH3:2][O:3][C:4]1[CH:9]=[C:8]([S:10]([Cl:13])(=[O:12])=[O:11])[CH:7]=[CH:6][C:5]=1[C:14]1[NH:15][C:16]2[C:17]([N:22]=1)=[N:18][CH:19]=[CH:20][CH:21]=2.COC1C=C(S(Cl)(=O)=O)C=CC=1C(O)=O.[CH3:38][NH:39][CH3:40]>>[ClH:13].[CH3:2][O:3][C:4]1[CH:9]=[C:8]([S:10]([N:39]([CH3:40])[CH3:38])(=[O:12])=[O:11])[CH:7]=[CH:6][C:5]=1[C:14]1[NH:15][C:16]2[C:17]([N:22]=1)=[N:18][CH:19]=[CH:20][CH:21]=2Komponenten
4
Versuchsvorschrift
The crude 2-(2'-methoxy-4'-chlorosulfonyl-phenyl)-imidazo[4,5-b]pyridine hydrochloride prepared from 2.5 gm of 2-methoxy-4-chlorosulfonyl-benzoic acid according to Example C was added to 150 ml of a saturated aqueous dimethylamine solution at 10° C., under stirring, and a light-colored precipitate formed slowly. After stirring for 20 hours at ambient temperature, 200 ml of ice water were added. The precipitate was dried and then taken up in 60 ml of methanol, and 10 ml of methanolic hydrochloric acid were added. After filtering over active charcoal, the solvent was eliminated, and the residue remaining was digested with acetone and ether, subjected to suction filtration, and washed with ether.
Aufarbeitung
- customa light-colored precipitate formed slowly
- stirringAfter stirring for 20 hours at ambient temperature
- customThe precipitate was dried
- addition10 ml of methanolic hydrochloric acid were added
- filtrationAfter filtering over active charcoal
- filtrationsubjected to suction filtration
- washwashed with ether
Quellen und Nachweise
- ORD-Eintrag
- ord-b0531ecf3c564a98af57cd6405a0dd48
- Quelldatensatz
- uspto-grants-1987_09
- Patentnummer
- US04696931
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