1-(3-BroMophenyl)-3-(diMethylaMino)-2-propen-1-one synthesis

Yield:163852-04-8 55.1%

Reaction Conditions:

in 5,5-dimethyl-1,3-cyclohexadiene; for 21 h;Reflux;

Steps:

7.1; 9.1 Step 1:
Preparation of 1-(3-bromo-phenyl)-3-dimethylamino-prop-2-en-1-one

10.0 g of 3-bromoacetophenone (50.2 mmol, 1.0 equiv.), 18.0 g of N, N-dimethylformamide dimethylacetal (150.7 mmol, 3.0 equiv.), and 50 ml of xylene were refluxed overnight (21 hours), a little raw material was not reacted and the reaction was stopped.
The reaction solution was cooled and concentrated to remove xylene.
150 ml of petroleum ether was added to the residue, and a solid precipitated under stirring, followed by filtration to obtain 7.0 g of 1-(3-bromo-phenyl)-3-dimethylamino-prop-2-en-1-one as a yellow solid, 55.1%.

References:

EP3287456,2018,A1 Location in patent:Paragraph 0077; 0091