* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Synthesis of the compound 25 The compound 24 (10g, 0.065 mol) was added into 100 mL of water, a concentrated sulphuric acid (12 mL) was slowly added with agitation and cooled to 0 °C in an ice bath. Sodium nitrite (6.9 g, 0.098 mol) was added in batches, reacted at 0°C for 4h, and left standing for 12 h. A large amount of yellow precipitate was precipitated, filtrated under the reduced pressure, vacuum-dried to obtain 7.7 g of a yellow product with a yield of 77percent. The melting point is 216.5-218.5°C (water).
Reference：
[1] Patent: EP2366691, 2011, A1, . Location in patent: Page/Page column 11
[2] Journal of the American Chemical Society, 1952, vol. 74, p. 3828,3830
2
[ 21901-29-1 ]
[ 39745-39-6 ]
[ 56057-19-3 ]
Reference：
[1] Journal of the American Chemical Society, 1947, vol. 69, p. 63,66
[2] Journal of Heterocyclic Chemistry, 1996, vol. 33, # 6, p. 1815 - 1821
[3] Journal of the American Chemical Society, 1947, vol. 69, p. 63,66
[4] Journal of Heterocyclic Chemistry, 1996, vol. 33, # 6, p. 1815 - 1821
With sulfuric acid; water; sodium nitrite; at 0℃; for 16h;
Synthesis of the compound 25 The compound 24 (10g, 0.065 mol) was added into 100 mL of water, a concentrated sulphuric acid (12 mL) was slowly added with agitation and cooled to 0 C in an ice bath. Sodium nitrite (6.9 g, 0.098 mol) was added in batches, reacted at 0C for 4h, and left standing for 12 h. A large amount of yellow precipitate was precipitated, filtrated under the reduced pressure, vacuum-dried to obtain 7.7 g of a yellow product with a yield of 77%. The melting point is 216.5-218.5C (water).
A. 2-Hydroxy-5-nitro-6-methylpyridine To a suspension of a 2:1 mixture of 2-amino-5-nitro-6-methylpyridine and 2-amino-3-nitro-6-methylpyridine (2.5 g, 16.3 mmol) in 15 mL of water at 0 C. was added concentrated sulfuric acid (5 mL), followed by a solution of NaNO2 (2.25 g, 32.6 mmol) in 5 mL of water dropwise over 90 minutes. The solution was stirred 5 hours as it warmed to room temperature, cooled to 0 C. and filtered. The solid was washed with water (2*) and dried under vacuum to afford 1.84 g of a >4:1 mixture (by HPLC) of Compound A and <strong>[39745-39-6]2-hydroxy-3-nitro-6-methylpyridine</strong> (73%) as a tan solid.
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