Preparation method for Mitiglinide calcium hydrate
A mitiglinide calcium and reaction technology, which is applied in the field of medicine, can solve problems such as being unsuitable for industrial production, and achieve high industrial production value, mild reaction conditions, and high yield.
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[0028] Add cis-hexahydroisoquinoline (250.4g, 2mol), anhydrous potassium carbonate (304.0g, 2.2mol), dichloromethane (1000ml) into the reaction flask, keep the temperature at 0-5°C, and stir vigorously, Add a solution of chloroacetyl chloride (271.0g, 2.4mol) in dichloromethane (500ml) dropwise, after the drop, react at room temperature for 2.5h, spot plate monitoring, after the reaction is complete, add 1000ml of water, separate the organic layer, wash with water (1000ml), Wash with saturated brine (1000ml), dry with anhydrous sodium sulfate overnight, distill off dichloromethane under reduced pressure to obtain cis-N-chloroacetylhexahydroisoindole (2) 357.4g oil, yield: 88.6%.
[0029] cis-N-chloroacetylhexahydroisoindole (302.5g, 1.5mol), N-phenylpropionylcamphorsultam (573.0g, 1.65mol), 70% sodium hydride (56.6g, 1.65mol), N,N-Dimethylformamide (900ml) was added into the reaction flask, and stirred vigorously at 50°C for 12h to obtain an alkylated product, which was kept a...
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