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103474-01-7

Benzeneacetic acid, α-oxo-2-phenoxy-, methyl ester synthesis

3synthesis methods
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Yield:103474-01-7 80%

Reaction Conditions:

Stage #1: diphenyletherwith n-butyllithium in Petroleum ether at -15; for 1 h;Inert atmosphere;
Stage #2: Dimethyl oxalate in Petroleum ether; for 2 h;Solvent;Reagent/catalyst;

Steps:

1.1

1) First, diphenyl ether (20g, 0.12mol), petroleum ether 100mL, added to a 250mL three-necked bottle under nitrogen protection, cooled to -15 ° C,The n-butyllithium solution was added dropwise while maintaining the temperature. After the addition was completed, the reaction was kept for 1 hour, then dimethyl oxalate was added dropwise, and the reaction was carried out for 2 hours, and then neutralized at -5 ° C with 10% hydrochloric acid to neutralize.This was washed successively with water, extracted, dried and distilled to obtain 21.7 g of the intermediate methyl 2-(2-phenoxyphenyl)-2-oxoacetate, content 95%, yield 80%.

References:

CN108129349,2018,A Location in patent:Paragraph 0028; 0039; 0044; 0046; 0048; 0050