3-Cyano-6-hydroxypyridone SodiuM Salt synthesis
- Product Name:3-Cyano-6-hydroxypyridone SodiuM Salt
- CAS Number:91467-46-8
- Molecular formula:C6H4N2NaO2
- Molecular Weight:158
Yield:91467-46-8 88.5%
Reaction Conditions:
with sodium methylate in methanol at 45 - 50; for 6 h;
Steps:
2; 4 Example 2
0055] 160 g of 1,3-dibenzyluracil, 55.2 g of cyanoacetamide (1.2 eq), 256.6 g of sodium methoxide solution (2.5 eq), and 800 mL of methanol were placed in a 2000 L reaction flask, and stirring was started. The temperature is raised to 45~50 ° C, and the reaction is kept for 6 hours.After the TLC detection reaction was completed, the reaction solution was cooled to 20 to 30 ° C, suction filtered, and the filter cake was rinsed with an appropriate amount of methanol. A filter cake and 800 g of water were placed in a 2000 L reaction flask.The temperature was raised to 70~75 ° C, then slowly cooled to 0~5 ° C for 2 h, and filtered, and the filter cake was rinsed with an appropriate amount of ice water to obtain sodium 3-cyano-2,6-dihydroxypyridine dihydrate. 94.0g, yield 88.5%, HPLC purity 99.6%, its TGA spectrum is shown in Figure 1, its HPLC spectrum is shown in Figure 2, and its 1 NMR spectrum is shown in Figure 5.
References:
CN108341771,2018,A Location in patent:Paragraph 0053-0055; 0059-0061
