Method for preparing nicergoline intermediate by using microchannel reactor
A nicergoline, microreactor technology, applied in chemical instruments and methods, chemical/physical/physical chemical reactors, chemical/physical/physical chemical processes, etc., to achieve high conversion rate and selectivity, simple process, product good quality effect
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Embodiment 1
[0037] Weigh 1.0 g of concentrated sulfuric acid and dissolve it in 10.0 g of methanol, stir at room temperature to make it evenly mixed to form a homogeneous solution A. Weigh 10.0 g of ergot alcohol, dissolve it in 50 ml of methanol, stir at room temperature to make it evenly mixed to make homogeneous solution B. The homogeneous solution A and the homogeneous solution B are pumped into the Y-type mixer with the flow velocity of 0.20ml / min and 0.80ml / min respectively, pass into the microreactor of 1mm after mixing, and the ultraviolet lamp irradiation reaction ( HPLR-N 250W Philips UV lamp, 330nm), the reactor volume is 5mL, the reaction temperature is controlled at -15°C, and the reaction residence time is 20min. The effluent from the micro-reaction device was collected, and the conversion rate was calculated by HPLC, and the conversion rate was 92.3%. Most of the solvent was evaporated, 50ml of water was added, filtered, and dried to obtain 10.4g of crude 10α-methoxy-photo...
Embodiment 2
[0039] Weigh 1.0 g of concentrated sulfuric acid and dissolve it in 10.0 g of methanol, stir at room temperature to make it evenly mixed to form a homogeneous solution A. Weigh 10.0 g of ergot alcohol, dissolve it in 50 ml of methanol, stir at room temperature to make it evenly mixed to make homogeneous solution B. The homogeneous solution A and the homogeneous solution B are pumped into the Y-type mixer with the flow rate of 0.40ml / min and 1.60ml / min respectively, pass into the microreactor of 1mm after mixing, and the ultraviolet lamp irradiation reaction ( HPLR-N 250W Philips UV lamp, 330nm), the reactor volume is 5mL, the reaction temperature is controlled at -15°C, and the reaction residence time is 20min. The effluent from the micro-reaction device was collected, and the conversion rate was calculated by HPLC, and the conversion rate was 90.5%. Most of the solvent was evaporated, 50ml of water was added, filtered, and dried to obtain 10.2g of crude 10α-methoxy-photoergool...
Embodiment 3
[0041] Weigh 10.0 g of concentrated sulfuric acid and dissolve it in 100.0 g of methanol, stir at room temperature to make it evenly mixed to form a homogeneous solution A. Weigh 100.0 g of ergot alcohol, dissolve it in 500 ml of methanol, stir at room temperature to make it evenly mixed to make homogeneous solution B. The homogeneous solution A and the homogeneous solution B are pumped into the Y-type mixer with the flow velocity of 0.20ml / min and 0.80ml / min respectively, pass into the microreactor of 1mm after mixing, and the ultraviolet lamp irradiation reaction ( HPLR-N 250W Philips UV lamp, 330nm), the reactor volume is 5mL, the reaction temperature is controlled at -15°C, and the reaction residence time is 20min. The effluent from the micro-reaction device was collected, and the conversion rate was calculated by HPLC, and the conversion rate was 93.0%. Most of the solvent was evaporated, 50ml of water was added, filtered, and dried to obtain 104.7g of crude 10α-methoxy-...
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