HRID277985

反应详情

EQUATION

反应方程式

HRID 277985 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a suspension of 2-amino-5-nitro-6-methylpyridine (40.24 g, 260 mmol) was added concentrated sulfuric acid (48 mL). The homogeneous solution was cooled to 0° C., and sodium nitrate (26.97 g, 390 mmol) dissolved in 120 mL of water was added. The reaction mixture was warmed to room temperature over 4 hours, then cooled to 0° C. The resulting ivory precipitate was collected, washed with cold water, and dried at 40° C. in vacuo overnight to provide 39.05 g (97%) of the title compound. EA calculated for C6H6N2O3: C, 46.76; H, 3.92; N, 18.18. Found: C, 46.49; H, 3.94; N, 17.99.

WORKUP

后处理

  1. additionwas added
  2. temperatureThe reaction mixture was warmed to room temperature over 4 hours
  3. temperaturecooled to 0° C
  4. customThe resulting ivory precipitate was collected
  5. washwashed with cold water
  6. customdried at 40° C. in vacuo overnight