反应详情

温度

0 °C

3 ml of 1,1,2,3,3,3-hexafluoropropanesulfonic acid were added to a solution of 20 ml of tetrahydrofuran (THF) and 4.2 g of 9-ethyl-3-carbazolylamine. After cooling to 0° C., 3 ml of isoamyl nitrite were added dropwise while stirring in such a way that the temperature did not rise above 10° C. After completion of the dropwise addition, the icebath was removed and the stirring of the reaction mixture was continued for a further 4 h. 50 ml of diethyl ether were added, and the precipitate produced was filtered off by suction, washed with a little diethyl ether and dried. 7.4 g of 9-ethyl-3-carbazolediazonium 1,1,2,3,3,3-hexafluoropropanesulfonate was obtained as a yellow, finely crystalline powder.

1. customdid not rise above 10° C
2. additionAfter completion of the dropwise addition
3. customthe icebath was removed
4. stirringthe stirring of the reaction mixture
5. addition50 ml of diethyl ether were added
6. customthe precipitate produced
7. filtrationwas filtered off by suction
8. washwashed with a little diethyl ether
9. customdried