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Ethanone, 2-chloro-1-(1-naphthalenyl)- (9CI) synthesis

6synthesis methods
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Yield:76469-33-5 60%

Reaction Conditions:

with aluminum (III) chloride in 1,2-dichloro-ethane at 10 - 15; for 3 h;Inert atmosphere;

Steps:

2 Synthesis of raw material 3B:

After venting nitrogen into a three-necked reaction flask equipped with a stirrer, a thermometer, and a constant pressure dropping funnel, add 80.0 mL of dichloroethane, raw material 3B-1 (50 mmol), anhydrous aluminum trichloride (60 mmol), and reduce the temperature to 10 ~15°C, add 2-chloroacetyl chloride (55 mmol) dropwise. After dripping, keep the reaction for 3 hours, add 100 mL of water, separate the liquids, extract the aqueous phase with 80.0 mL of dichloroethane, combine the organic phases, wash twice with 100 mL of water each time. The organic phase was dried with 5g of anhydrous sodium sulfate, the organic phase was concentrated at (3540, -0.04-0.06MPa) until no drips flowed out, and recrystallized with dichloromethane: petroleum ether=1:5 to obtain the raw material 3B (30mmol), yield 60%.

References:

CN111171028,2020,A Location in patent:Paragraph 0072-0075