反应详情

A stirred mixture of 4-(1H-1,2,4-triazol-1-yl)phenol (16.1 g, 0.10 mole), 2-chloroethanol (25.5 g, 0.30 mole), potassium carbonate (42 g, 0.30 mole) and methyl ethyl ketone (100 ml) was heated at reflux temperature for 10 hr. An additional 16.1 g (0.20 mole) of 2-chloroethanol was added to the reaction mixture and heating at reflux temperature continued for another 24 hr. The hot mixture was filtered and the filtrate chilled. The crystalline precipitate was collected by filtration and the filter cake rinsed with water to remove most of the dark color. The solid was triturated with hot ethyl acetate, the mixture cooled, and the light-tan crystals collected to yield 14.0 g (68%), mp 151°-152° C.

1. temperaturewas heated
2. temperatureat reflux temperature for 10 hr
3. temperatureheating
4. temperatureat reflux temperature
5. filtrationThe hot mixture was filtered
6. temperaturethe filtrate chilled
7. filtrationThe crystalline precipitate was collected by filtration
8. washthe filter cake rinsed with water
9. customto remove most of the dark color
10. customThe solid was triturated with hot ethyl acetate
11. temperaturethe mixture cooled
12. customthe light-tan crystals collected
13. customto yield 14.0 g (68%), mp 151°-152° C.