Sodium Azide → HCID 178468987、化合物
反応式
[C:1]([C:6]1[CH:11]=[CH:10][C:9]([N:12]=[C:13]=[S:14])=[CH:8][CH:7]=1)([O:3][CH2:4][CH3:5])=[O:2].[N-:15]=[N+:16]=[N-:17].[Na+]>O>[C:1]([C:6]1[CH:11]=[CH:10][C:9]([N:12]2[C:13]([SH:14])=[N:17][N:16]=[N:15]2)=[CH:8][CH:7]=1)([O:3][CH2:4][CH3:5])=[O:2]参加物
4
反応条件
- 温度
- 80 °C
実験手順
20 g of 4-carboethoxyphenyl isothiocyanate and 6.5 g of sodium azide are added to water and heated at 80° C. After 2 hours of reaction, the reaction mixture is filtered, cooled and acidified with hydrochloric acid to give crystals of 1-(4-carboethoxyphenyl)-5-mercaptotetrazole. To the crystals are added 5 equivalents of sodium hydroxide (1N NaOH in water) and the mixture is heated at 80° C. for 5 hours. After cooling, the reaction mixture is acidified with hydrochloric acid to cause crude crystals of Compound III-4 to separate out. The crystals are recrystallized from methanol. Yield: 55%, m.p. about 195° C. (decomposed).