Dimethylamine → HCID 14373876, compound

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Reaction Conditions

Reaction Steps

Next, 37% aqueous formaldehyde solution and DMF are added into a reactor. The reactor is cooled to 0-5° C. and 33% aqueous dimethylamine solution then is added slowly with stirring. Concentrated sulfuric acid is added slowly to the mixture while the temperature is maintained at below 10° C. The mixture is stirred for an additional 15 minutes and cooled to 0-5° C. A solution of 5,6-dichloroindole (C) in DMF is added slowly to the reactor and stirred for an additional hour at 0-5° C. The mixture is allowed to warm to room temperature and stirred for 24 hrs. The mixture is then added to a reactor containing a solution of industrial sodium chloride in water. Activated carbon next is added and the mixture stirred for 30 minutes. Upon filtration, the filtrate is adjusted to pH>12 with 20% aqueous sodium hydroxide solution. The precipitate is filtered, washed with water until pH=7-8, centrifuged, and dried to yield crude 5,6-dichlorogramine (D). Recrystallization in 70% ethanol produces the pure product with melting point of 150-154° C.

Provenance & Evidence