反应详情

温度

-40 °C

1200 ml of anhydrous DMF are initially charged in a 4 l reaction flask and cooled to −40° C. At this temperature, 336.5 g (4.56 mol) of potassium methoxide (95%) are added with stirring and suspended. A mixture of 300 g (1.92 mol) of 3-nitro-o-xylene (97%) and 274 g (2.52 mol) of n-butyl nitrite (95%) is subsequently added dropwise at −40° C. over a period of 7 hours (if the mixture is cooled appropriately, the duration of this addition can be reduced at will; an extension has hitherto not been examined; temperature variations between −35 and −45° C. can be tolerated). By HPLC, it is checked that the starting material has been converted completely. The reaction discharge is subsequently added with stirring to a mixture of 300 ml of water and 300 ml of glacial acetic acid, at from −5 to 0° C. The reaction mixture is then poured into 6 kg of ice-water and the solid is separated off by filtration (without any problems, the flow resistance has not yet been determined) and washed twice with 500 ml of water each time (caution: the crude product smells strongly). The crude product (HPLC: 96 area %) is purified by suspending the moist solid in 800 ml of toluene for 1.5 h. The solid is filtered off (without any problems, the flow resistance has not yet been determined) and dried in a vacuum drying cabinet at 50° C.

1. additionis subsequently added dropwise at −40° C. over a period of 7 hours (if the mixture
2. temperatureis cooled appropriately
3. additionthe duration of this addition
4. customtemperature variations between −35 and −45° C.
5. additionThe reaction discharge is subsequently added
6. customthe solid is separated off by filtration (without any problems
7. washwashed twice with 500 ml of water each time (caution
8. customThe crude product (HPLC: 96 area %) is purified
9. customfor 1.5 h
10. filtrationThe solid is filtered off (without any problems
11. customdried in a vacuum
12. customdrying cabinet at 50° C.