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858445-94-0

ETHYL 4-(2,4-DIMETHOXYPHENYL)-4-OXOBUTYRATE synthesis

3synthesis methods
-

Yield:-

Reaction Conditions:

with aluminum (III) chloride in 1,2-dichloro-ethane at 0 - 20; for 1 h;

Steps:

72 Synthesis of Compound 2

Ethyl succinyl chloride (18 g, 0.11 mol) dissolved in 1.2-DCE (1000 ml), the reaction mixture cooled to 0° C., AlCl3 (17.3 g, 0.13 mol) added dropwise with stirring at 0° C., the above suspension added a solution of compound 1 (13.8 g, 0.1 mol) in 200 ml of 1,2-DCE from the dropping funnel over a period of 30 min, the mixture solution stirred at RT for 30 min, TLC (PE:EA=1:1) showed the starting material was consumed completely. The above solution poured into 1000 ml ice-water, the organic layers separated, the aqueous layer was extracted with DCM (500*3), the combined organic layers were washed with sat NaCl (500 ml*2), dried over Na2SO4, the solvent was removed to get the crude compound 2 (16 g, 60%) and use at the next step directly.

References:

JP2015/214548,2015,A Location in patent:Paragraph 1245; 1246

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