Reaktionsgleichung
[OH-].[K+].[CH3:3][O:4][C:5]1[CH:6]=[C:7]2C(=[CH:12][C:13]=1[O:14][CH3:15])NC=[CH:8]2.[I:16]I.IC.S([O-])([O-])(=O)=S.[Na+].[Na+].[CH3:27][N:28]([CH3:31])[CH:29]=O>O>[I:16][C:8]1[C:7]2[C:27](=[CH:12][C:13]([O:14][CH3:15])=[C:5]([O:4][CH3:3])[CH:6]=2)[N:28]([CH3:31])[CH:29]=1Komponenten
Edukt 6
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 5 °C
Versuchsvorschrift
0.465 g of powdered potassium hydroxide is added to a solution of 0.5 g of 5,6-dimethoxy-1H-indole in 15 ml of dimethylformamide. A solution of 0.725 g of bisublimated iodine in 15 ml of dimethylformamide is added dropwise to the above mixture. After agitation of the reaction medium for approximately 3 hours at a temperature in the region of 20° C., 0.21 ml of iodomethane is added dropwise, maintaining the mixture at this same temperature by cooling using a water bath. After agitation at around 20° C. for 1 hour 30 minutes, the mixture is run into a solution of 1.5 g of sodium thiosulfate in 150 ml of water cooled to around 5° C., and agitated for approximately 10 minutes. The precipitate is filter-dried, washed with five times 5 ml of water cooled to around 5° C., and then dried under vacuum (13 kPa) over phosphorus pentaoxide. 0.78 g of 3-iodo-5,6-dimethoxy-1-methyl-1H-indole is obtained in the form of a solid, the characteristics of which are as follows:
Aufarbeitung
- temperaturemaintaining the mixture at this same temperature
- temperatureby cooling
- customThe precipitate is filter-dried
- washwashed with five times 5 ml of water
- temperaturecooled to around 5° C.
- dry with materialdried under vacuum (13 kPa) over phosphorus pentaoxide
Quellen und Nachweise
- ORD-Eintrag
- ord-d8b6e25a6b8e41cba01926c0db395b78
- Quelldatensatz
- uspto-grants-2011_06
- Patentnummer
- US07968566B2
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