6-苯基-5-氯-3(2H)-哒嗪酮合成工艺的改进

Improvement of synthesis process for 6-phenyl-5-chloro-3-pyridazone

6-苯基-3-哒嗪酮经三氯化磷和氯气氯代,所得中间体6-苯基-3,5-二氯哒嗪经氢氧化钠皂化、盐酸酸化制得标题化合物,通过回收皂化反应的副产物6-苯基-3-氯-5-羟基哒嗪作为氯代反应的原料,总收率56.6%,考察了回收物料及氯气流量对氯代反应的影响,讨论了皂化产物的分离工艺,最终产物经1HNMR结构确证。

6-Phenyl-5-chloro-3（2H）-pyridazone was synthesized from 6-phenyl-3-pyridazone by chlorination with chlorine and phosphorus trichloride to give 3-phenyl-4,6-dichloropyridazine which saponified with sodium hydroxide,followed by acidified with HCl,the overall yield is 56.6% by recycling isomer 6-phenyl-3-chloro-5-hydroxylpyridazine from saponifination as raw material used in chlorination.Effects of recycled by-product and flow rate of chlorine in chlorination on yield were investigated,separation procedure of saponification was discussed,the structure of the target product was confirmed by 1HNMR.