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75302-98-6

ACEMETACINTERT-BUTYLESTER synthesis

2synthesis methods
-

Yield:75302-98-6 95.7%

Reaction Conditions:

with N-benzyl-N,N,N-triethylammonium chloride;sodium carbonate in toluene at 75; for 45 h;Large scale;

Steps:

1 Preparation of acemetacin tert-butyl ester

850kg of toluene and 48kg of tert-butyl chloroacetate were pumped into the reaction tank in sequence, 100kg of indomethacin, 35kg of sodium carbonate, and 8kg of benzyltriethylammonium chloride were sequentially added, and the temperature was raised to 75°C with stirring, and the reaction was kept warm for 4 hours.Add 300kg of water, stir for 10 minutes, and separate into layers.Add 300 kg of water to the organic phase, stir for 10 minutes, and separate into layers.The organic phase was distilled under reduced pressure to remove the toluene, the temperature was reduced to room temperature, 400kg of methanol was added, the temperature was refluxed until the solution was clear, the temperature was lowered to crystallize, spin filtration, and drying at 80°C to obtain 126kg of acemetacin tert-butyl ester with a yield of 95.7%. HPLC content: 99.62%.

References:

CN111960986,2020,A Location in patent:Paragraph 0010

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