HRID379476

反应详情

EQUATION

反应方程式

HRID 379476 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

Combine methyl 2-methoxy-5-aminobenzoate (3.94 g, 21.7 Limol) and triethyl orthoformate (12.8 g, 86.7 mmol) in glacial acetic acid (20 mL). After 20 hours, concentrate the reaction mixture in vacuo to remove ethanol. Add glacial acetic acid (20 mL) and sodium azide (5.64 g, 86.7 mmol). Heat to 70° C. After 1 hour, add glacial acetic acid (10 mL) and continue to heat to 70° C. After an additional hour, cool the reaction mixture to ambient temperature, dilute with water (500 mL). Collect the solid by filtration, rinse with water, and dry to give methyl 2-methoxy-5-(1H-tetrazol-1-yl)benzoate.

WORKUP

后处理

  1. concentrationconcentrate the reaction mixture in vacuo
  2. customto remove ethanol
  3. waitAfter 1 hour
  4. temperatureto heat to 70° C
  5. waitAfter an additional hour
  6. temperaturecool the reaction mixture to ambient temperature
  7. customCollect the solid
  8. filtrationby filtration
  9. washrinse with water
  10. customdry