反应详情

20 g of 4-aminophenol (Mw=109.13; 0.18324 mol) are suspended in 200 cm3 of anhydrous dichloromethane, under an inert atmosphere. The suspension is cooled to a temperature of 0° C. in a bath of ice and 16.4 cm3 of anhydrous pyridine (Mw=79.10; d=0.981; 0.2034 mol) are then added. 17.6 cm3 of ethyl chloroformate (Mw=108.53; d=1.13; 0.18324 mol) are then added dropwise so as to keep the mixture at a temperature below 10° C. The reaction mixture is kept stirring for two hours. The mixture is poured onto one liter of ice-cold water and then extracted with ethyl acetate. The organic phase is washed with water and then dried, filtered and evaporated under vacuum. After recrystallization from a heptane/ethyl acetate mixture, 21 g of a white powder are obtained, which corresponds to a yield of 63%. The melting point of the product obtained is 127.2° C. The H NMR spectrum and the elemental analysis are in accordance with the expected product.

1. additionare then added
2. customat a temperature below 10° C
3. extractionextracted with ethyl acetate
4. washThe organic phase is washed with water
5. customdried
6. filtrationfiltered
7. customevaporated under vacuum
8. customAfter recrystallization from a heptane/ethyl acetate mixture, 21 g of a white powder
9. customare obtained
10. customThe melting point of the product obtained
11. customis 127.2° C