Reaktionsgleichung
Br[CH2:2][CH:3]1[O:17][C:6]2=[C:7]3[C:12](=[C:13]([CH3:15])[CH:14]=[C:5]2[CH2:4]1)[NH:11][C:10](=[O:16])[CH:9]=[CH:8]3.[CH3:18][N:19]([CH2:21][CH2:22][SH:23])[CH3:20].[OH-].[Na+]>CN(C)C=O.Cl.O>[CH3:18][N:19]([CH3:20])[CH2:21][CH2:22][S:23][CH2:2][CH:3]1[O:17][C:6]2=[C:7]3[C:12](=[C:13]([CH3:15])[CH:14]=[C:5]2[CH2:4]1)[NH:11][C:10](=[O:16])[CH:9]=[CH:8]3Komponenten
7
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 3
Versuchsvorschrift
To a suspension of 2-bromomethyl-5-methyl-2,3,6,7-tetrahydrofuro-[2,3-f]quinoline-7-one (1. 765 g) in dimethylformamide (60 ml), hydrochloric acid salt of 2 (dimethylamino)ethylmercaptan (4.25 g) and caustic soda (2.40 g) in water (20 ml) were added and stirred at room temperature for 1 hour. The solvent was distilled off under reduced pressure. The residue was combined with water, and extracted with chloroform. The extract was washed with NaCl solution twice and dried and condensed. The residue was crystallized from chloroform--n-hexane to obtain 1.741 g of the title compound as white powder (mp.: 163°-165° C.).
Aufarbeitung
- additionwere added
- distillationThe solvent was distilled off under reduced pressure
- extractionextracted with chloroform
- washThe extract was washed with NaCl solution twice
- customdried
- customcondensed
- customThe residue was crystallized from chloroform
Quellen und Nachweise
- ORD-Eintrag
- ord-9c5b9c9f1a514ec1a9a9042f54391201
- Quelldatensatz
- uspto-grants-1996_11
- Patentnummer
- US05576324
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