Refining method of pentazocine
A technology of pentazocine and its refining method, which is applied in the field of purification of chemical drugs, can solve the problems of long treatment time, poor color, and low yield of the purification process, and achieve the effects of low equipment requirements, good color, and high purity
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Embodiment 1
[0020] The preparation of embodiment 1 pentazocine crude product
[0021] Add 6kg of 5,9-dimethyl-2'-hydroxyl-6,7-benzomorphinane, 70L of N-methylpyrrolidone and 4.8kg of potassium bicarbonate into a 100L glass-lined reactor, slowly add 1 - 5.2kg of bromo-3-methyl-2-butene, slowly heated up to 80°C for 6 hours. After the reaction is completed, transfer to the extraction tank after cooling to room temperature, add 70L of 28% salt water, and extract with 70L and 40L of chloroform in turn, after combining the organic phases, wash them twice with 50L of purified water, and then combine the organic phases for heating Concentrate to dryness, add 60L methyl tert-butyl ether and concentrate again to dryness, add 80L methyl tert-butyl ether, heat and dissolve until clear, cool to below 10°C, add 18L of 2N HCl diethyl ether solution dropwise, and obtain pentamethasone The crude Zocine hydrochloride was vacuum-dried at 30-35°C to obtain 8.80kg of light yellow solid.
[0022] Add 200L o...
Embodiment 2
[0023] The refining of embodiment 2 pentazocine crude product
[0024] After mixing 8L of acetone and 2L of water evenly, heat to 50°C, add 1 kg of crushed fine powder of pentazocine crude product, pass the fine powder through an 80-mesh sieve, continue heating to reflux, and stir for half an hour. Filtrate while it is hot at a filtration temperature of 60°C, and vacuum-dry the filter cake (temperature at 50°C, vacuum degree -0.08Mpa) to obtain 0.92kg of pentazocine refined product, with a yield of 92%; the content is greater than 99.1% after analysis and detection. The mother liquor is distilled under normal pressure, and 7.3 L of acetone can be recovered, with a recovery rate of 91%.
Embodiment 3
[0025] The refining of embodiment 3 pentazocine crude product
[0026] After mixing 7L of methanol and 2L of water evenly, heat to 55°C, add 1 kg of fine powder of the crude pentazocine that has been pulverized, pass the fine powder through a 300-mesh sieve, continue heating to reflux, and stir for half an hour. Filtrate while it is hot at a filtration temperature of 60°C, and vacuum-dry the filter cake (at a temperature of 70°C, at a vacuum of -0.09Mpa) to obtain 0.91kg of a refined product of pentazocine, with a yield of 91%. The content is greater than 99.2% through analysis and detection. The mother liquor was distilled under normal pressure, and 6.5 L of methanol could be recovered, with a recovery rate of 93%.
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