Preparation method of norepinephrine
A technology of methylepinephrine and methanol, applied in the field of preparation of norepinephrine, can solve the problems of long process steps, complicated operation, low recovery rate, etc., and achieve the effect of simple steps, high purity and low cost
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Embodiment 1
[0052] Add 210.28g of urotropine, 1200ml of chloroform, 250g of SSXS-0, and 1000ml of isopropanol to a 5000ml four-necked flask with a drying tube at 25 degrees, heat the reaction system to 63 degrees, keep the temperature for 4 hours, TLC Monitor the completion of the reaction, cool down to 25°C and stir for 1 hour, filter out the solid, rinse with 500ml of acetone, and dry at 50°C. The 410g product SSXS-1 is directly used in the next step without purification. Yield 93.65%, if figure 1 shown.
[0053] Add 120g of SSXS-1, 862.5ml of methanol, and 194.4ml of concentrated hydrochloric acid to the 4-port cake with a drying tube, heat the reaction system to 60-65 degrees, keep the temperature for 3-4 hours, TLC monitors the completion of the reaction, and then cool down after the completion of the reaction To 25 degrees, adjust the pH to be neutral, solids are precipitated, filter the solids, rinse with water, dry at 50 degrees, and obtain 72g of product SSXS-2 after salt format...
Embodiment 2
[0057] A preparation method of norepinephrine, which comprises the following steps:
[0058] (1) Add urotropine, chloroform, SSXS-0 and isopropanol at 22°C, then react at 65°C for 3.5 hours, then cool down to 23°C and stir for 0.95 hours, filter out the solid, and rinse with washing liquid 1 Wash and dry to obtain SSXS-1;
[0059] (2) Mix SSXS-1, methanol and concentrated hydrochloric acid and react at 63.5°C for 3.5 hours. After the reaction is completed, cool down to 25°C and adjust the pH to neutral. Solids are precipitated. Filter the solids and rinse with pure water and dry to obtain SSXS -2;
[0060] (3) Add SSXS-2, palladium / carbon and methanol to the hydrogenation device, replace the gas and heat to 45°C, keep hydrogenation at 4.2 atmospheres for 5.2 hours, cool down to 8°C after the reaction is completed, and pass ammonia gas into the reaction solution The pH value of the solution was 9.32, and the precipitated solid was filtered, rinsed with washing solution 2, and...
Embodiment 3
[0075] A preparation method of norepinephrine, which comprises the following steps:
[0076] (1) Add urotropine, chloroform, SSXS-0 and isopropanol at 23°C, then react at 65°C for 3.5 hours, then cool down to 23°C and stir for 0.98 hours, filter out the solid, and rinse the solid with washing solution 1 Wash and dry to obtain SSXS-1;
[0077] (2) Mix SSXS-1, methanol and concentrated hydrochloric acid, react at 64°C for 3.5 hours, cool down to 25°C after the reaction is completed, adjust the pH to neutral, and solids precipitate out, filter the solids, rinse with pure water, and dry to obtain SSXS -2;
[0078] (3) Add SSXS-2, palladium / carbon and methanol to the hydrogenation device, replace the gas and heat to 45°C, keep hydrogenation at 4.2 atmospheres for 5.5 hours, cool down to 8°C after the reaction is completed, and pass ammonia gas into the reaction solution The pH value of the solution was 9.35, and the precipitated solid was filtered, rinsed with washing liquid 2, a...
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