Preparation method of quinoline, isoquinoline and various kinds of methyl quinoline
A technology of methylquinoline and isoquinoline, which is applied in the direction of organic chemistry, can solve the problems of unrecycled and utilized waste, long process flow, and high production cost, so as to improve the utilization rate of raw materials, simple process flow, and high production cost. low cost effect
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Embodiment 1
[0037] Embodiment 1 of the present invention discloses a preparation method of quinoline, isoquinoline and various methylquinolines, specifically comprising the following steps:
[0038] (1) thiourea is dissolved in water to form a mass concentration of 3% thiourea solution;
[0039] (2) Mix the isoquinoline residue with the above-mentioned thiourea solution evenly, and react for 5 hours at a temperature of 20° C. and 800 r / min stirring conditions, and filter and dry to obtain a white solid product after the reaction is completed;
[0040] (3) Ethanol, propanol, methyl ethyl ketone and pentanone are configured into a mixed solvent according to the mass ratio of 22:10:9:8, and then the white solid product is added according to the solid-to-liquid ratio of 1:2, stirred evenly, and filtered to obtain Filtrate and thiourea coronal clathrate:
[0041] (4) cooling and crystallizing the above-mentioned filtrate at 1° C., and then undergoing solid-liquid separation to obtain 2,4-dime...
Embodiment 2
[0044] Embodiment 2 of the present invention discloses a preparation method of quinoline, isoquinoline and various methylquinolines, specifically comprising the following steps:
[0045] (1) thiourea is dissolved in water to form a mass concentration of 8% thiourea solution;
[0046] (2) Mix the isoquinoline residue with the above-mentioned thiourea solution evenly, and react for 2 hours at a temperature of 30° C. and 500 r / min stirring conditions, and filter and dry to obtain a white solid product after the reaction is completed;
[0047] (3) Ethanol, propanol, methyl ethyl ketone and pentanone will be configured into a mixed solvent according to the mass ratio of 25:8:11:6, and then the white solid product will be added according to the solid-to-liquid ratio of 1:5 and stirred evenly, after filtration, respectively Obtain filtrate and thiourea coronal clathrate;
[0048] (4) cooling and crystallizing the above-mentioned filtrate at 3° C., and then undergoing solid-liquid sepa...
Embodiment 3
[0051] Embodiment 3 of the present invention discloses a preparation method of quinoline, isoquinoline and various methylquinolines, specifically comprising the following steps:
[0052] (1) thiourea is dissolved in water to form a mass concentration of 5% thiourea solution;
[0053] (2) Mix the isoquinoline residual liquid with the above-mentioned thiourea solution evenly, and react for 3.5 hours at a temperature of 25° C. and 650 r / min under stirring conditions. After the reaction is completed, filter and dry to obtain a white solid product;
[0054] (3) Ethanol, propanol, methyl ethyl ketone and pentanone will be configured into a mixed solvent according to the mass ratio of 23:9:10:7, and then the white solid product will be added according to the solid-to-liquid ratio of 1:4 and stirred evenly, after filtration, respectively Obtain filtrate and thiourea coronal clathrate;
[0055] (4) cooling and crystallizing the above-mentioned filtrate at 2° C., and then undergoing so...
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