Synthesis method of 6-methyl nicotine
A technology of methyl nicotine and synthesis method, which is applied in the direction of organic chemistry, can solve the problems of difficult separation of 6-methyl nicotine, unfixed methyl substitution position, harsh reaction conditions, etc., so as to avoid difficult separation, poor selectivity, conditionally controlled effects
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Embodiment 1
[0051] The synthesis route of 6-methylnicotine of the present embodiment is as follows:
[0052] The specific operation steps are as follows:
[0053] S1. Weigh 800mg of γ-butyrolactone (9.3mmol) and dissolve it in 150ml of N,N-dimethylformamide (DMF), cool down to 0°C, stir for 10min, then add 240mg of NaH (9.9mmol) in batches, and react After 30 min, 1 g of methyl 6-methylnicotinate (6.6 mmol) was added, the refrigeration was turned off, and the reaction was carried out at room temperature for 5 h, and the end point was determined by TLC detection to obtain compound I;
[0054] S2. First add a small amount of 5w% dilute hydrochloric acid to compound I until no bubbles are generated, then add 20ml concentrated hydrochloric acid and 20ml 1,4-dioxane, heat to 95°C and react for 5h, after the complete reaction of compound I is determined by TLC detection, Cool down to room temperature, add 50% NaOH solution under ice bath conditions to adjust the pH to 9, combine the organic ph...
Embodiment 2
[0060] S1. Weigh 800mg of γ-butyrolactone (9.3mmol) and dissolve it in 150ml of tetrahydrofuran, cool down to 0°C, stir for 10min, then add 240mg of NaH (9.9mmol) in batches, react for 30min, then add 1g of 6-methylnicotinic acid Methyl ester (6.6mmol), turn off the refrigeration, react at room temperature for 5h, and determine the end point by TLC detection to obtain compound I;
[0061] S2. First add a small amount of 5w% dilute hydrochloric acid to compound I until no bubbles are generated, then add 20ml concentrated hydrochloric acid and 20ml 1,4-dioxane, heat to 95°C and react for 5h, after the complete reaction of compound I is determined by TLC detection, Cool down to room temperature, add 50% NaOH solution under ice bath conditions to adjust the pH to 9, combine the organic phases after extraction and concentrate and dry to obtain compound II;
[0062] S3. Compound II was dissolved in 20ml of methanol, 250mg of sodium borohydride was added, and reacted at -10°C for 2 h...
Embodiment 3
[0066] S1. Weigh 800mg of γ-butyrolactone (9.3mmol) and dissolve it in 150ml of tetrahydrofuran, cool down to 0°C, stir for 10min, then add 960mg of sodium tert-butoxide (9.9mmol) in batches, react for 30min, then add 1g of 6-methanol Nicotinic acid methyl ester (6.6 mmol), turn off the refrigeration, react at room temperature for 5h, and determine the end point by TLC detection to obtain compound Ⅰ;
[0067] S2. First add a small amount of 5w% dilute hydrochloric acid to compound I until no bubbles are generated, then add 20ml concentrated hydrochloric acid and 20ml 1,4-dioxane, heat to 95°C and react for 5h, after the complete reaction of compound I is determined by TLC detection, Cool down to room temperature, add 50% NaOH solution under ice bath conditions to adjust the pH to 9, combine the organic phases after extraction and concentrate and dry to obtain compound II;
[0068] S3. Compound II was dissolved in 20ml of methanol, 250mg of sodium borohydride was added, and rea...
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