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ChemicalBook CAS DataBase List 4-chloro-4'-methoxybenzophenone

4-chloro-4'-methoxybenzophenone synthesis

13synthesis methods
Obtained by reaction of 4-chlorobenzoyl chloride with anisole in the presence of –MoO2Cl2 (20 mol%) at reflux for 20 h (75%).
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Yield:10547-60-1 99%

Reaction Conditions:

with tert.-butylnitrite;oxygen;acetic acid;2,3-dicyano-5,6-dichloro-p-benzoquinone in 1,1,2,2-tetrachloroethane at 130; for 12 h;Autoclave;

Steps:

2 3.2 A typical procedure for DDQ/TBN-catalyzed aerobic oxidation of diarylmethanes

General procedure: A Teflon-lines 316 L stainless steel autoclave (300 mL) equipped with magnetic stirring bar was charged with substituted diarylmethanes 1 (2 mmol), 136.2 mg DDQ (0.6 mmol, 30 mol %), 41.2 mg TBN (0.4 mmol, 20 mol %), 480 mg acetic acid (8 mmol) and 20 mL TeCA. The autoclave was closed and charged with oxygen to 0.3 MPa. Then the autoclave was placed in an oil bath, which was preheated to 130 °C. The mixture was then stirred for a certain time until the reaction was completed. The autoclave was taken out from the oil bath, cooled to room temperature and carefully depressurized. The mixture was concentrated under reduced pressure and purified by column chromatography to give the desired diarylketones.

References:

Ma, Jiaqi;Hu, Zhiming;Li, Meichao;Zhao, Weijuan;Hu, Xinquan;Mo, Weimin;Hu, Baoxiang;Sun, Nan;Shen, Zhenlu [Tetrahedron,2015,vol. 71,# 38,p. 6733 - 6739]

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