反应详情

温度

22.5 °C

143.6 g (1 mole) of 2-amino-4-chlorphenol was suspended in 550 ml of methyl t-butyl ether under mild nitrogen purge. The mixture was heated to reflux until the material was dissolved. After 40 minutes, 112.3 g of acetic anhydride was added. After the addition the mixture was cooled to 20-25° C. in one hour. After stirring for an additional hour the mixture was cooled to 0-5° C. under stirring and kept on this temperature for an additional hour. The product was filtered off, washed with 200 ml of methyl t-butyl ether twice and dried at 50° C. and 100 mbar under a gentle nitrogen stream till dry. Yield about 92%.

1. custompurge
2. temperatureThe mixture was heated
3. temperatureto reflux until the material
4. dissolutionwas dissolved
5. addition112.3 g of acetic anhydride was added
6. additionAfter the addition the mixture
7. temperaturewas cooled to 0-5° C.
8. stirringunder stirring
9. waitkept on this temperature for an additional hour
10. filtrationThe product was filtered off
11. washwashed with 200 ml of methyl t-butyl ether twice
12. customdried at 50° C.
13. customtill dry