Manufacturing method for a piperidine-3-ylcarbamate compound and optical resolution method therefor
A kind of carbamate, the technology of the production method, applied in the production of piperidin-3-yl carbamate compound and the field of optical separation, can solve problems such as unsatisfactory industry, achieve the effect of cheap production
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Embodiment 1
[0152] Embodiment 1: the manufacture of pyridin-3-ylcarbamate isopropyl ester
[0153] In a solution obtained by dissolving 50.0 g (0.53 mol) of 3-aminopyridine and 8.94 g (0.11 mol) of sodium bicarbonate in 150 ml of water, 75.7 g (0.61 mol) of isopropyl chlorocarbonate was added dropwise in parallel over 2 hours. and 230 ml of a 15% by weight potassium hydroxide aqueous solution. The internal temperature of the mixture in dripping was maintained at 0-10 degreeC, and pH was maintained at 7-8. After the dropwise addition, the obtained mixture was stirred at room temperature for 1 hour, and the precipitated crystals were filtered and washed with 200 ml of water. The obtained crystals were dried to obtain 89.3 g of isopropyl pyridin-3-ylcarbamate. The yield was 93.3%.
Embodiment 2
[0154] Embodiment 2: the manufacture of piperidin-3-ylcarbamate isopropyl ester
[0155] 17.9 g of palladium carbon (5%) was added to a solution obtained by dissolving 89.3 g (0.50 mol) of isopropyl pyridin-3-ylcarbamate obtained in Example 1 in 178.6 g (2.97 mol) of acetic acid, and Stir at 0.5 MPa and 70° C. for 14 hours. After the reaction, the palladium carbon was separated by filtration to obtain a reaction solution, and the palladium carbon was washed with 225 ml of water to obtain a washing liquid, and the reaction solution and the washing liquid were mixed. The obtained solution was added dropwise to a solution obtained by dissolving 119 g (2.98 mol) of sodium hydroxide in 129 ml of water. The internal temperature of the mixture during dropwise addition was maintained at 0 to 10°C. The obtained mixture was extracted with 180 ml of tert-butyl methyl ether, and the obtained organic layer was dried over magnesium sulfate. Magnesium sulfate was separated by filtration, ...
Embodiment 3
[0158] Embodiment 3: the manufacture of piperidin-3-ylcarbamate isopropyl ester
[0159] Suspend 60 g (0.33 mol) of isopropyl pyridin-3-ylcarbamate obtained in the same manner as in Example 1 in 90 mL of water, add 30 g (0.50 mol) of acetic acid, and then add palladium carbon (5%) 3.0 g, the obtained mixture was stirred for 23 hours under the conditions of hydrogen pressure 0.5Mpa and 90°C. After the reaction, 100 mL of 1-butanol was added to the reaction mixture, and palladium carbon was filtered to obtain a reaction solution. Palladium carbon was washed with 20 mL of 1-butanol to obtain a washing liquid, and the above reaction solution and washing liquid were mixed. A solution obtained by dissolving 20.0 g (0.50 mol) of sodium hydroxide in 47 mL of water was added dropwise to the obtained solution at 20 to 25° C., stirred, and an organic layer was obtained by liquid separation treatment. The aqueous layer was extracted with 120 mL of 1-butanol, and the obtained organic lay...
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