反应详情

温度

120 °C

Under a dry nitrogen atmosphere 4.1 g (0.0021 mole) of 3-chloro-4-phenyl-1,2,5-thiadiazole was added to a stirred mixture of 3.73 g (0.0027 mole) of potassium carbonate and 2.4 g (0.0026 mole) of phenol in 50 ml of N,N-dimethylformamide. After complete addition the mixture was heated at 120° C. for 21 hours. The mixture was cooled, poured into 400 ml of ice water and the mixture extracted with diethyl ether. The extract was dried over anhydrous magnesium sulfate and filtered. The filtrate was evaporated under reduced pressure to leave a residue. The residue was purified by column chromatography on silica gel, eluted with n-hexane:methylene chloride (1:1) to yield 4.8 g of 3-phenoxy-4-phenyl-1,2,5-thiadiazole, Compound 38 of Table I.

1. additionAfter complete addition the mixture
2. temperatureThe mixture was cooled
3. extractionthe mixture extracted with diethyl ether
4. dry with materialThe extract was dried over anhydrous magnesium sulfate
5. filtrationfiltered
6. customThe filtrate was evaporated under reduced pressure
7. customto leave a residue
8. customThe residue was purified by column chromatography on silica gel
9. washeluted with n-hexane:methylene chloride (1:1)