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ChemicalBook CAS DataBase List 2-Benzyl-2-(dimethylamino)-4'-morpholinobutyrophenone
119313-12-1

2-Benzyl-2-(dimethylamino)-4'-morpholinobutyrophenone synthesis

9synthesis methods
Morpholine

110-91-8

1-Butanone, 2-(dimethylamino)-1-(4-fluorophenyl)-2-(phenylmethyl)-

119312-61-7

2-Benzyl-2-(dimethylamino)-4'-morpholinobutyrophenone

119313-12-1

General procedure for the synthesis of 2-benzyl-2-dimethylamino-1-P-fluorophenyl-1-butanone from 2-benzyl-2-dimethylamino-1-P-fluorophenyl-1-butanone and morpholine: 2-benzyl-2-dimethylamino-1-P-fluorophenyl-1-butanone was dissolved in ethylene dichloride and transferred to a four-necked flask. Morpholine (139.6 g, 1.6 mol) and 1 L of dichloroethane were added and the reaction was heated to reflux state. The reaction progress was monitored by TLC or high performance liquid chromatography (HPLC). After completion of the reaction, the reaction was cooled to room temperature, the reaction mixture was washed by adding 200 ml of water and stirred for 30 min. After standing and layering, the organic phase was separated. The solvent was recovered by distillation under reduced pressure to obtain the crude product. The crude product was recrystallized from 440 ml of ethanol to give 117.2 g of a light yellow solid product with a melting point of 115-116 °C, an overall yield of 80% and a purity of 99.3%.

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Yield:119313-12-1 85%

Reaction Conditions:

in 1,2-dichloro-ethaneReflux;Solvent;

Steps:

9 Example 9; preparation of 2-benzyl-2-dimethylamino-1-(4-morpholino phenyl)-1-butanone
take 2-benzyl-2-dimethylamino-1-P-fluorophenyl-1-butanone dissolve in dichloroethane solution and add morpholine (139.6g, 1 . 6mol) into 1L in four-mouth bottle, heating reflux reaction, TLC or liquid phase chromatographic monitoring reaction, after the reaction is complete, reducing the temperature to room temperature, add 200 ml water washing, stirring 0.5h, layering, the organic phase is separated, and recovering the solvent, by residues 440 ml ethanol is recrystallized to get pale yellow solid 117.2, melting point: 115-116°C, the overall yield is 80%, purity 99.3%

References:

Shandong Chemical Technology Co., Ltd. day long;Zhang, Qi;Luo, Xian;Wu, Rui;Wang, Tao;Lui, Changwei;Li, Yilin;Li, Hongzhou;Li, Ke;Luzhen, Bo;Zhao, Guofeng CN105384707, 2016, A Location in patent:Paragraph 0003; 0034

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