ChemicalBook CAS DataBase List Acemetacin

Acemetacin synthesis

6synthesis methods

Product Name:Acemetacin
CAS Number:53164-05-9
Molecular formula:C21H18ClNO6
Molecular Weight:415.82

alkylation of indomethacin with benzyl bromoacetate in K2CO3/N,N-dimethylformamide gives the corresponding benzyl glycolate ester, which is hydrogenated over 10 % palladium on charcoal in acetic acid to yield acemetacin.

75302-98-6 Synthesis

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53164-05-9
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Yield:53164-05-9 99.45%

Reaction Conditions:

with hydrogenchloride;acetic anhydride in acetic acid at 80; for 5 h;Large scale;

Steps:

2-5 Preparation of acemetacin
Put 250kg of acetic acid into the reaction tank, and pass hydrogen chloride with stirring until the content of hydrogen chloride (w/w) is 12%.Add 2.04 kg of acetic anhydride with a mass of 6% by mass of hydrogen chloride and stir evenly, and then add 100 kg of acemetacin tert-butyl ester,Control the temperature at 80°C and stir for 5 hours, then lower the temperature to 20°C, and let stand for 2 hours until the crystallization is complete.After suction filtration, top washing, and drying at 80°C, 84.2 kg of asemexine was obtained, with a yield of 95.59%.Dissolve the crude product in 360kg of toluene, heat it to clear, add 1kg of activated carbon,Stir for 20 minutes, filter with suction, cool to room temperature, and let stand for 2 hours until crystallization is complete.Filtered, washed with a small amount of toluene, drained, and dried at 80°C to obtain 83.74 kg of acemetacin.The refined yield is 99.45%, and the HPLC content is 99.88%.

References:

Henan Dongtai Pharmaceutical Co., Ltd.;Miao Qing;Qian Weiguo;Li Taijun;Liu Wenqiang;Lu Yin;Song Xiaoxing;Li Wenguang CN111960986, 2020, A Location in patent:Paragraph 0002; 0011-0014

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75302-98-6 Synthesis

75302-98-6
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53-86-1 Synthesis