77470-80-5Relevant articles and documents
Synthesis method of anesthetic bupivacaine impurities
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Paragraph 0007; 0008, (2018/11/22)
The invention relates to a synthesis method of anesthetic bupivacaine impurities. The synthesis method comprises the following steps: (a) adding 6-bromocaproic acid, dichloromethane and N,N-dimethylformamide to a reaction container, dropwise adding oxalyl chloride under the conditions of ice salt bath and nitrogen protection, performing reaction at 0-25 DEG C after addition, performing concentration after the reaction, adding toluene for concentration again to obtain a 6-bromohexanoyl chloride crude product, dissolving the 6-bromohexanoyl chloride crude product in dichloromethane, dropwise adding a dichloromethane solution of dimethylaniline under the conditions of ice salt bath and nitrogen protection, performing reaction at 5-10 DEG C after addition, and performing direct filtering, washing and drying after the reaction to obtain a compound ii; (b) adding the compound ii, n-butylamine, potassium carbonate and acetonitrile to another reaction container for reaction at 30-50 DEG C, andpurifying a product after reaction to obtain the anesthetic bupivacaine impurities. The anesthetic bupivacaine impurities prepared from 6-bromocaproic acid and oxalyl chloride as raw materials are set as drug quality standards by the European Pharmacopoeia, and the method has the advantages of simple process and convenient reaction steps.
