精细与专用化学品
精細與專用化學品
정세여전용화학품
FINE AND SPECIALTY CHEMICALS
2012年
6期
39-42
,共4页
陈再新%夏正君%蒋龙%林送%王彬%张明光%王明林
陳再新%夏正君%蔣龍%林送%王彬%張明光%王明林
진재신%하정군%장룡%림송%왕빈%장명광%왕명림
1-环丙基-6，7-二氟1，4-二氢-4-氧3喹啉羧酸%喹诺酮%中间体%合成
1-環丙基-6，7-二氟1，4-二氫-4-氧3喹啉羧痠%喹諾酮%中間體%閤成
1-배병기-6，7-이불1，4-이경-4-양3규람최산%규낙동%중간체%합성
1-eyelopropyl 6,7-difluoro-1,4-dihydro-4-oxo 3-quinolone carboxylic acid%quinolone%intermedi ate%synthesis
以2，4，5三氟苯甲酸为原料，氯代后与丙二酸二乙酯缩合，经硫酸水解得2，4，5三氟苯甲酰乙酸乙酯，再与原甲酸三乙酯缩合，不经纯化，与环丙胺反应后，得到2-（2，4，5三氟苯甲酰基）3-环丙胺基丙烯酸乙酯，再在氟化钠的催化下环合后，水解得到目标产物1环丙基-6，7二氟-1，4-二氢4-氧-3-喹啉羧酸，总收率68．6％。
以2，4，5三氟苯甲痠為原料，氯代後與丙二痠二乙酯縮閤，經硫痠水解得2，4，5三氟苯甲酰乙痠乙酯，再與原甲痠三乙酯縮閤，不經純化，與環丙胺反應後，得到2-（2，4，5三氟苯甲酰基）3-環丙胺基丙烯痠乙酯，再在氟化鈉的催化下環閤後，水解得到目標產物1環丙基-6，7二氟-1，4-二氫4-氧-3-喹啉羧痠，總收率68．6％。
이2，4，5삼불분갑산위원료，록대후여병이산이을지축합，경류산수해득2，4，5삼불분갑선을산을지，재여원갑산삼을지축합，불경순화，여배병알반응후，득도2-（2，4，5삼불분갑선기）3-배병알기병희산을지，재재불화납적최화하배합후，수해득도목표산물1배병기-6，7이불-1，4-이경4-양-3-규람최산，총수솔68．6％。
1-Cyclopropyl-6,7-difluoro-1,4-dihydro 4-oxo-3-quinolone carboxylic acid was synthesized from 2, 4, 5-trifluorobenzoie acid, which was subjected to thionyl chloride in toluene, then condensed with diethyl mal- onate, and hydrolyzed by sulfuric acid in water gave the β-keto ester. The β-keto ester was allowed to react with triethyl orthoformate in acetic anhydride followed by treatment with an equimolar amount of cyclopropylamine gave predominantly the enamino ketoester, followed by cyclization with sodium fluoride and hydrolysis by acids gave the target product with an overall yield of about 68.6%.
