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709025-22-9

1-(4-bromo-2-methylphenyl)propan-1-one synthesis

3synthesis methods
178313-45-6 Synthesis
4-bromo-N-methoxy-N,2-dimethylbenzamide

178313-45-6
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1-(4-bromo-2-methylphenyl)propan-1-one

709025-22-9
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Yield:709025-22-9 86 %

Reaction Conditions:

in tetrahydrofuran at 0 - 20;

Steps:

1.2 2. The synthesis of intermediate 1.3

[0630] To a stirred solution of 1.2 (4.0 g, 15.6 mmol) in dry THF (20 mL) was slowly added ethylmagnesium bromide (2.0 M/THF, 15.5 mL, 31.0 mmol) at 0 °C. The reaction mixture was stirred at RT for 2 h. Saturated NH4CI (a.q.) was added and the mixture was extracted with EA (30 mL x 2), the organic layer was washed with water, dried over anhydrous Na2SO4 and evaporated to dryness. The crude product was purified by prep-HPLC to give 1.3 (3.0 g, yield: 86%) as yellow oil. LC-MS m/z: 227.1 [M+H]+.

References:

WO2022/167457,2022,A1 Location in patent:Paragraph 0629-0630