Aceclofenac tert-butyl ester synthesis
- Product Name:Aceclofenac tert-butyl ester
- CAS Number:139272-68-7
- Molecular formula:C20H21Cl2NO4
- Molecular Weight:410.29
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Yield:139272-68-7 94.45%
Reaction Conditions:
with potassium iodide in ethanol at 61 - 65; for 3 h;Large scale;Temperature;
Steps:
1.1; 2.1; 2.1; 3.1
(1) Add 2.5 kg of ethanol to a 10L reactor, stir and heat,Add 2.25kg diclofenac sodium, 1.8kg tert-butyl bromoacetate (1.3eq),The catalyst potassium iodide is 0.082kg (0.07eq), and then 0.6kg of ethanol is added to flush the material pipe.Warm up to 61-65, start to keep warm, and start sampling and testing after 3 hours.When the content of diclofenac sodium in the liquid phase is about 2%, the reaction is complete.After the heating is stopped, the temperature is reduced to 10°C, and then it can be filtered. Add 2kg of water to rinse the materials to wash away the salts.After drying, 2.74 kg of Aceclofenac tert-butylester can be obtained, with a purity of 99.28% and a yield of 94.45%.
References:
CN111848426,2020,A Location in patent:Paragraph 0021-0022; 0025-0026; 0032-0033; 0036-0037
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139272-68-7
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