A kind of preparation method of 5-cyano-3-(4-chlorobutyl)-indole
A technology of chlorobutyl and cyanophenyl, which is applied in the field of preparation of 5-cyano-3-indole, can solve the problems of difficult source of raw materials, high yield of waste water, etc., and achieves short preparation process route and low cost , the effect of short synthetic route
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Embodiment 1
[0029] The preparation of embodiment 1 zinc reagent
[0030] Add 13g (0.2mol) of zinc powder to a dry round bottom flask, heat to 70°C under vacuum and continue the vacuum for 3 hours, then put nitrogen, then add 0.95g (0.04mol) of iodine and 150mL tetrahydrofuran or N, N-dimethylacetamide, the reaction solution was stirred until the red color of iodine faded, and then 29.9 g (0.15 mol) of newly distilled 6-chlorobromohexane was added, and the resulting mixture was heated and reacted at 60 ° C for 5 h, and the sample was analyzed. Until the raw material 6-chlorobromohexane is completely reacted. The obtained gray solution is directly used for the next step reaction. The zinc reagent is stable and does not decompose when stored under a nitrogen atmosphere at room temperature for several weeks. The reaction solution is diluted with anhydrous tetrahydrofuran or anhydrous N,N-dimethylacetamide to obtain Zinc reagent solution at a concentration of 2.0M.
Embodiment 2
[0031] The preparation of embodiment 2 zinc reagents
[0032] Add 13g (0.2mol) of zinc powder to a dry round bottom flask, heat to 70°C under vacuum and continue the vacuum for 3 hours, then put nitrogen, then add 0.95g (0.04mol) of iodine and 150mL tetrahydrofuran or N, N-dimethylacetamide, the reaction solution was stirred until the red color of iodine faded, and then 29.9 g (0.15 mol) of newly distilled 6-chlorobromohexane was added. The obtained mixture was heated and reacted at 40° C. for 24 h, and samples were taken for analysis until the raw material 6-chlorobromohexane was completely reacted. The obtained gray solution is directly used for the next step reaction. The zinc reagent is stable and does not decompose when stored under a nitrogen atmosphere at room temperature for several weeks. The reaction solution is diluted with anhydrous tetrahydrofuran or anhydrous N,N-dimethylacetamide to obtain Zinc reagent solution at a concentration of 2.0M.
Embodiment 3
[0033] The preparation of embodiment 3 zinc reagents
[0034] Add 13g (0.2mol) of zinc powder to a dry round bottom flask, heat to 70°C under vacuum and continue the vacuum for 3 hours, then put nitrogen, then add 0.95g (0.04mol) of iodine and 150mL tetrahydrofuran or N, N-dimethylacetamide, the reaction solution was stirred until the red color of iodine faded, and then 29.9 g (0.15 mol) of newly distilled 6-chlorobromohexane was added. The obtained mixture was heated and reacted at 100° C. for 15 h, and samples were taken for analysis until the raw material 6-chlorobromohexane was completely reacted. The obtained gray solution is directly used for the next step reaction. The zinc reagent is stable and does not decompose when stored under a nitrogen atmosphere at room temperature for several weeks. The reaction solution is diluted with anhydrous tetrahydrofuran or anhydrous N,N-dimethylacetamide to obtain Zinc reagent solution at a concentration of 2.0M.
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