1029-24-9Relevant academic research and scientific papers
Synthesis method of dilazep drug intermediate 3-chloropropyl 3,4,5-trimethoxybenzoate
-
Paragraph 0014; 0015, (2016/11/21)
The invention relates to a synthesis method of a dilazep drug intermediate 3-chloropropyl 3,4,5-trimethoxybenzoate, which comprises the following steps: adding 0.81 mol of 3,4,5-trimethoxybenzoic acid, 1.51-1.53 mol of 1-amino-3-chloropropane and 1.3L of acetonitrile into a reaction vessel which is provided with a stirrer and a reflux condenser, heating the solution to 60-65 DEG C, refluxing for 3-5 hours, adding 0.52 mol of sodium sulfite solution in batches, reacting for 14-15 hours while keeping the stirring rate at 130-170 rpm, cooling the solution to 10-15 DEG C, filtering, distilling the filtrate under reduced pressure, recovering the solvent, adding 500ml of cyclohexane into the residue, heating the solution to 70-75 DEG C, keeping for 90-120 minutes, cooling to separate crystals out, carrying out suction filtration, washing with a salt solution, washing with ethyl acetate, dehydrating with a dehydrating agent, and recrystallizing in propionitrile to obtain the crystal 3-chloropropyl 3,4,5-trimethoxybenzoate.
