N-Butyl-3-cyano-6-hydroxy-4-methyl-2-pyridone synthesis
- Product Name:N-Butyl-3-cyano-6-hydroxy-4-methyl-2-pyridone
- CAS Number:39108-47-9
- Molecular formula:C11H14N2O2
- Molecular Weight:206.24
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Yield: 237 g
Reaction Conditions:
Stage #1:N-butylamine;methyl 2-cyanoacetate at 100; for 5 h;
Stage #2:acetoacetic acid methyl ester with piperidine at 100; for 5 h;
Steps:
1
200 g of methyl cyanoacetate and 136 g of butylamine were mixed,After stirring at 100 ° C. for 5 hours, 226 g of methyl acetoacetate,Subsequently, 181 g of piperidine was added dropwise and the mixture was stirred at 100 ° C. for 5 hours.After cooling the reaction solution to room temperature, the reaction solution was added dropwise to 2000 g of 7.2 wt% hydrochloric acid vigorously stirred.The precipitate obtained by filtration was stirred and washed with 400 g of acetone / 600 g of water,After filtration, it was dried by heating under vacuum to obtain 237 g of compound (a).
References:
NIPPON SHOKUBAI COMPANY LIMITED;SHINGUBARA, KOJI;TATSUMI, HIRONORI;KITAMURA, MORIHIRO;MASUDA, KIYOSHI JP5727321, 2015, B2 Location in patent:Paragraph 0128; 0130; 0131
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