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29681-99-0

1-(2-METHOXY-PHENYL)-BUTANE-1,3-DIONE synthesis

3synthesis methods
-

Yield:29681-99-0 75%

Reaction Conditions:

with sodium amide at 60;Claisen Condensation;

Steps:

4 4.2. General procedure for the preparation of 8

General procedure: The starting material 7 (60 mmol) was dissolved in EtOAc(26.5 g, 300 mmol). After stirring for 10 min, NaNH2 (4.68 g,120 mmol) was subsequently added, followed allowing the reactionto stir for 0.5 h at room temperature. Then, the mixture wasgradually heated up to 60 C. After stirring for 5-8 h, the reactionmixture was gradually allowed to reach room temperature and30 mL of HCl (1 M) was added. The mixture was extracted withEtOAc (30 mL 3) and the combined organic layers were driedover sodium sulfate, filtered and concentrated to dryness. The productwas purified over silica gel using ethyl acetate: petroleum(1:1) to obtain the product 8.

References:

Yan, Jun;Hu, Jinhui;Liu, Anqiu;He, Lin;Li, Xingshu;Wei, Hui [Bioorganic and Medicinal Chemistry,2017,vol. 25,# 12,p. 2946 - 2955]

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