New method for preparation of duloxetine hydrochloride
A technology of duloxetine hydrochloride and duloxetine, which is applied in the field of duloxetine hydrochloride preparation, and can solve problems such as incomplete hydrolysis, affecting product purity, and difficulty in oil purification
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Embodiment 1
[0019] Example 1: Preparation of Duloxetine from Methyl Duloxetine:
Embodiment 1-1
[0020] Example 1-1: Add 5.0 g (16.1 mmol) of methyl duloxetine, 60 mL of methanol and 12.0 mL of 0.15M sodium acetate-sodium hydroxide buffer (pH=8.0) to the reaction flask, stir at room temperature, and add Iodine 5.3 g (20.9 mmol), heated at 50 ℃ and stirred for 3.5 hours. After the reaction is complete, methanol is evaporated under reduced pressure, 30 mL of 0.5M sodium sulfite solution is added, extracted with dichloromethane (50 mL×3), dried with sodium sulfate and evaporated to dryness Deduloxetine oil 4.2 g, yield 91.6%, content 98.7% (area normalization method).
Embodiment 1-2
[0021] Example 1-2: Add 5.0 g (16.1 mmol) of methyl duloxetine, 60 mL of acetone and 60 mL of 0.1M potassium dihydrogen phosphate-potassium hydroxide buffer (pH=10.0) to the reaction flask, at 20°C Under stirring, 8.2 g (32.2mmol) of iodine was added and stirred at 20°C for 6 hours. After the reaction was completed, the acetone was evaporated under reduced pressure, and 50 mL of 0.5M sodium bisulfite solution was added, and extracted with ethyl acetate (50 mL×3). After drying with sodium sulfate and evaporating to dryness, 4.3 g of duloxetine oil was obtained, with a yield of 89.5% and a content of 93.4% (area normalization method).
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