HRID1388675
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionTo a mixture of 8.2 g
- customevaporated to dryness
- washThe residue was washed with dilute hydrochloric acid
- customrecrystallized from N,N-dimethylformamide
- dissolutiondissolved in base
- filtrationfiltered
- customreprecipitated
- additionwith dilute acid
- filtrationfiltered
- washwashed with methanol
- customrecrystallized again from N,N-dimethylformamide