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THYLSULFANYL-PHENYL)-ACETIC ACID synthesis

4synthesis methods
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Yield:3583-58-2 80%

Reaction Conditions:

with tris-(dibenzylideneacetone)dipalladium(0);N-ethyl-N,N-diisopropylamine;4,5-bis(diphenylphosphino)-9,9-dimethylxanthene in 1,4-dioxane;Inert atmosphere;Reflux;

Steps:

1.1 step 1:Synthesis of 2-(4-(ethylthio)phenyl)acetic acid

Add 2-(4-bromophenyl)acetic acid (8.22 g, 38.2 mmol) to a 250 mL single-necked bottle, Xantphos(1.17 g, 2.0 mmol), N,N-diisopropylethylamine (13.4 mL, 76.4 mmol),1,4-Dioxane (100 mL), Pd2(dba)3 (887 mg, 0.96 mmol), ethanethiol (3.45 mL, 45.9 mmol) was added under argon.Heat to reflux overnight,The TLC test material has been reacted.The solvent was evaporated to give the crude product.Ethyl acetate = 1:1) gave a yellow solid product 5.95 g.The yield was 80.0%.

References:

CN109206346,2019,A Location in patent:Paragraph 0109; 0112; 0113; 0114; 0115; 0116