A simple and efficient method for synthesizing dinoprost
A dinoprost, high-efficiency technology, applied in the field of pharmaceutical preparation, can solve the problems of high cost, complicated operation, long steps, etc., and achieve the effect of increased reaction yield and simple operation
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[0060] The specific synthesis steps are as figure 1 Shown:
[0061] Step (1) Preparation of Compound I
[0062] In a 10L three-necked flask equipped with a constant pressure dropping funnel, a thermometer and a mechanical stirrer, respectively add Corinolidediol (500g, 2.907mol), DMN-AZADO (4.93g, 0.02907mol), and potassium bromide KBr (34.59). g, 0.2907mol), n-Bu4NBr (47.8g, 0.1454mol), dichloromethane (5L) and saturated sodium bicarbonate solution (400mL); then use an ice-salt bath for the above-mentioned mixed system, and cool to an internal temperature ≤0℃ , And stir at constant temperature for 10 min; then slowly add NaClO (3.4884 mol, used as oxidant) solution to the reaction system dropwise to control the reaction temperature not to be higher than 5°C; after the dropwise addition, stir at constant temperature for 30 minutes. After the reaction, add saturated Na to the system 2 S 2 O 3 (Neutralize excess oxidant) (1000 mL) The reaction was quenched, and the aqueous phase was...
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