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13735-09-6

Propanoic acid, 3-[(3-bromophenyl)thio]- synthesis

6synthesis methods
-

Yield:13735-09-6 500 mg

Reaction Conditions:

Stage #1: 3-bromobenzenethiolwith sodium hydroxide in lithium hydroxide monohydrate at 100; for 2 h;
Stage #2: 3-chloropropanoic acid in lithium hydroxide monohydrate at 60;

Steps:

9.1 Step 1: Preparation of 2-((3-bromophenyl)thio)propionic acid

m-bromothiophenol (0.27 mL) was dissolved in 5 mL of 2M aqueous sodium hydroxide solution, reacted at 100 °C for 2 h,The temperature of the reaction system was lowered to 60° C., 3-chloropropionic acid (302 mg) was added, and the reaction was carried out at 60° C. overnight. TLC monitored the reaction to complete.Cool to room temperature, adjust the pH of the system to 2 with 3M aqueous hydrochloric acid solution under ice bath, a large amount of solid is precipitated,After suction filtration, the filter cake was washed with water three times, and the filter cake was taken out and dried under reduced pressure to obtain the title compound (500 mg).

References:

CN114853814,2022,A Location in patent:Paragraph 0243-0248