反应详情

温度

47 °C

To a stirred, cooled (0° C.) dispersion of 1.52 g (0.00658 mol) of 5-chloromethoxy-4-hydroxy-2-nitrobenzaldehyde (10), 1 g AlCl3, and 10 ml dry dichloroethane, 2.4 ml of dry pyridine are added. During addition, the reaction mixture is protected from atmospheric moisture, and the temperature is kept below 35° C. When addition is complete, the temperature is raised to 47° C., and maintained for 18 hours. 6N HCl is added, keeping the temperature at 30°-35° C., until the mixture is acidic to Congo Red indicator paper. The acidic solution is extracted with diethyl ether, and the combined ether extracts are dried over Na2SO4. After filtration, the ether is removed at reduced pressure, giving 0.82 g (68%) of (1): mp 201°-202°° C.

1. additionare added
2. additionDuring addition
3. customis kept below 35° C
4. additionWhen addition
5. temperaturemaintained for 18 hours
6. customat 30°-35° C.
7. extractionThe acidic solution is extracted with diethyl ether
8. dry with materialthe combined ether extracts are dried over Na2SO4
9. filtrationAfter filtration
10. customthe ether is removed at reduced pressure