HRID1388675

反应详情

EQUATION

反应方程式

HRID 1388675 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

To a mixture of 8.2 g. of 3-methoxy-2-naphthoic acid, 5.2 g. of aminotetrazole, and 80 ml. of pyridine was added dropwise 6.4 ml. of thionyl chloride, maintaining the temperature below 70° C. After stirring for one hour, the mixture was cooled to 25° C. and evaporated to dryness. The residue was washed with dilute hydrochloric acid, then recrystallized from N,N-dimethylformamide, then dissolved in base, filtered, reprecipitated with dilute acid, filtered, washed with methanol, then recrystallized again from N,N-dimethylformamide to provide 3-methoxy-N-(tetrazol-5-yl)naphthalene-2-carboxamide (a type IV compound), m.p. 280°-283° C.

WORKUP

后处理

  1. additionTo a mixture of 8.2 g
  2. customevaporated to dryness
  3. washThe residue was washed with dilute hydrochloric acid
  4. customrecrystallized from N,N-dimethylformamide
  5. dissolutiondissolved in base
  6. filtrationfiltered
  7. customreprecipitated
  8. additionwith dilute acid
  9. filtrationfiltered
  10. washwashed with methanol
  11. customrecrystallized again from N,N-dimethylformamide