- Synthesis method of urapidil medical intermediate 1,3-dimethyl-6-(3-hydroxy propyl)aminouracil
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A synthesis method of a urapidil medical intermediate 1,3-dimethyl-6-(3-hydroxy propyl)aminouracil includes the following steps of adding 0.61 mol of 1,3-dimethyl-6-hydroxyl uracil (2), 0.72-0.75 mol of 3-amino-1-propanol and 0.16 mol of sodium sulfite solution to a reaction container provided with a stirrer, a thermometer and a reflux condenser, controlling the stirring speed at 130-160 rpm, raising the temperature of the solution to 150-160 DEG C, reacting for 90-120 min, lowering the temperature of the solution to 60-65 DEG C, adding 230 ml of cyclohexane, conducting refluxing for 30-50 min, conducting filtering, cooling filtrate to 5-9 DEG C, standing for 30-35 h, separating out crystals, conducting filtering, washing crystals with a saline solution and acetonitrile in sequence, conducting dehydration through a dehydrating agent, and conducting recrystallization in isopropanol to obtain white crystals 1,3-dimethyl-6-(3-hydroxy propyl)aminouracil.
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Paragraph 0014; 0015
(2016/11/21)
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