反应详情

温度

110 °C

0.48 g (1.8 mmol) of 5-bromo-2-pyrrolidin-1-yl-1H-benzimidazole and 34 mg (0.18 mmol) of CuI are placed in a round flask. The reaction vessel is flushed with argon. Then 0.54 g (3.6 mmol) of NaI, 32 mg (0.36 mmol) of dimethylenediamine, and 3 mL of 1,4-dioxane are added under argon. The reaction mixture is stirred for 14 hours at 110° C. Subsequently, the cooled reaction mixture is combined with concentrated ammonia solution, diluted with water, and the precipitate formed is filtered off. The solid is stirred with methanol and again filtered. Yield: 0.3 g (53% of theoretical); C11H12IN3 (M=313.13); calc.: molpeak (M+H)+: 314; found: molpeak (M)+: 314.

1. customThe reaction vessel is flushed with argon
2. customSubsequently, the cooled reaction mixture
3. customthe precipitate formed
4. filtrationis filtered off
5. stirringThe solid is stirred with methanol
6. filtrationagain filtered