4-Bromo-3-oxo-N-phenylbutanamide synthesis

5synthesis methods

Product Name:4-Bromo-3-oxo-N-phenylbutanamide
CAS Number:1205-74-9
Molecular formula:C10H10BrNO2
Molecular Weight:256.1

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62-53-3 Synthesis

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Yield: 93%

Reaction Conditions:

Stage #1:4-methyleneoxetan-2-one with bromine in dichloromethane at 5 - 15; for 1 h;
Stage #2:aniline in dichloromethane at 30 - 35; for 3 h;Solvent;Temperature;

Steps:

1-10
S1. Add 84g of diketene and 600g of organic solvent to the reaction flask, and cool to 5°C for stirring and mixing, then control the system temperature at 15°C,At the same time, 160 g of bromine was added dropwise for reaction to obtain a reaction liquid. among them,The organic solvent is dichloromethane;S2. After stirring the above reaction solution for 1 hour,120g of alkali was added for mixing, and then the temperature of the system was controlled at 30°C, while an appropriate amount of aniline was gradually added dropwise to react. After the drop was completed, the reaction was kept at 35°C for 3 hours to obtain the reaction product. Among them, the base is triethylamine;S3. After cooling the above reaction product to 3°C, it is filtered, and the filter cake is rinsed with 50g of dichloromethane, and then the filter cake is dried to obtain 4-bromo-3-oxo-N-phenyl Butanamide 238.2g.

References:

CN112321444, 2021, A Location in patent:Paragraph 0018-0029

102-01-2 Synthesis