Application of 70627-52-0, A common heterocyclic compound, 70627-52-0, name is N-(4-(Benzyloxy)benzylidene)-4-fluoroaniline, molecular formula is C20H16FNO, 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.
Preparation of TiCl4+Ti(O-i-Pr)4 mixed solution:The TiCl4 (21.3g, 0.112mol) dissolved in 100ml dichloromethane.Ti(O-i-Pr)4 (10.6 g, 0037 mol) was added dropwise at 0 C.The reaction was kept for 30 minutes.Intermediate A1-2 (53.4 g, 0.1 mol) andIntermediate A1-3 (61.4 g, 0.2 mol)Soluble in 250ml dichloromethane,DIPEA (25.8g, 0.2mol) was added dropwise at -15 C.TiCl4+Ti(O-i-Pr)4 mixed solution,After the addition is completed, the reaction is continued for 2 hours.Then glacial acetic acid (30 g, 0.5 mol) was added dropwise.After cooling in an ice bath, the reaction solution was poured into a 7% aqueous solution of tartaric acid.Stir for 1 h, naturally warm to room temperature,Add 100ml of 20% sodium bisulfite solution,Stirring was continued for 2 h, the organic layer was separated, washed with water, dried over anhydrous sodium sulfate, filtered, and concentrated.50 ml of methanol was beaten and the white solid was 62.1 g.
The synthetic route of 70627-52-0 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Wuxi Fuqi Pharmaceutical Co., Ltd.; Wang Qinglin; Wang Tao; Wang Binbin; Sun Yilin; (11 pag.)CN109369491; (2019); A;,
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