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ChemicalBook CAS DataBase List 1-(4-(Bromomethyl)phenyl)ethanone

1-(4-(Bromomethyl)phenyl)ethanone synthesis

5synthesis methods
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Yield:51229-51-7 95%

Reaction Conditions:

with N-Bromosuccinimide;2,2'-azobis(isobutyronitrile) in acetonitrile at 95; for 8 h;Inert atmosphere;

Steps:

5 preparation of intermediate A2
The preparative flow chart is shown in Fig.In a dry round-bottomed flask, 4 ml of p-methyl acetophenone was dissolved in 30 ml of dry acetonitrile,Under the protection of argon, 5.9 g of N-bromosuccinimide (NBS) and 500 mg of azobisisobutyronitrile (AIBN) were added,Continue under the protection of argon 95 ° C reflux 8h,Then cooled to room temperature and the solvent was dried under reduced pressure,The residue was dissolved in 40 ml of methylene chloride, and the organic phase was washed successively with 2M aqueous hydrochloric acid, saturated aqueous sodium hydrogencarbonate and saturated brine, then dried over anhydrous sodium sulfate and the solvent was dried under reduced pressure. The residue was recrystallized from petroleum ether: Ester = 30: 1 (volume ratio) over silica gel column,6 g of p-bromomethylacetophenone (colorless liquid) was obtained in a yield of 95%.

References:

TSINGHUA UNIVERSITY;RAO, YU;YANG, MAOJUN;YANG, YIQING;FENG, YUE CN103787966, 2016, B Location in patent:Paragraph 0115-0117

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