Synthetic Route of 455-75-4, A common heterocyclic compound, 455-75-4, name is Ethyl 3-amino-4-fluorobenzoate, molecular formula is C9H10FNO2, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
The 17.4g (94.9mmol) 3-amino-4-fluoro-benzoic acid ethyl ester (reference L.S.Fosdick, A.F.Dodds, J.Amer Chem.Soc. 65,2305 (1943)) and 9.67 ml (11.47g, 105 . 4mmol) methoxy acetyl chloride then 310 ml of chlorobenzene to the solution in the 50 C stirring 2 hours, then reflux 30 minutes. Concentrated under reduced pressure to dryness, purified by silica gel column chromatography (dichloromethane/ethanol = 100:1), oily product to be 3-amino-4-fluoro-benzoic acid ethyl ester, after a few days is cured into a solid (20.1g, yield 83%). R f value: 0.38 (silica gel: dichloromethane/ethanol = 19:1). Mass spectrometric (ESI-MS): 256.1(M+H) +, 278.1(M+Na) +; C 12 H 14 FNO 4 (255).
The synthetic route of 455-75-4 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Xizang Hai Sike Pharmaceutical Group Co., Ltd.; Li Qilin; Li Yue; Dang Juan; Long Yu; (53 pag.)CN103524559; (2016); B;,
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