Reaktionsgleichung
[F:1][C:2]([F:13])([S:9]([OH:12])(=[O:11])=[O:10])[CH:3]([F:8])[C:4]([F:7])([F:6])[F:5].[CH2:14]([N:16]1[C:28]2[CH:27]=[CH:26][C:25]([NH2:29])=[CH:24][C:23]=2[C:22]2[C:17]1=[CH:18][CH:19]=[CH:20][CH:21]=2)[CH3:15].[N:30](OCCC(C)C)=O>O1CCCC1>[F:13][C:2]([F:1])([S:9]([O-:12])(=[O:10])=[O:11])[CH:3]([F:8])[C:4]([F:5])([F:7])[F:6].[CH2:14]([N:16]1[C:28]2[CH:27]=[CH:26][C:25]([N+:29]#[N:30])=[CH:24][C:23]=2[C:22]2[C:17]1=[CH:18][CH:19]=[CH:20][CH:21]=2)[CH3:15]Komponenten
5
Reaktionsbedingungen
- Temperatur
- 0 °C
Versuchsvorschrift
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.
Aufarbeitung
- customdid not rise above 10° C
- additionAfter completion of the dropwise addition
- customthe icebath was removed
- stirringthe stirring of the reaction mixture
- addition50 ml of diethyl ether were added
- customthe precipitate produced
- filtrationwas filtered off by suction
- washwashed with a little diethyl ether
- customdried
Quellen und Nachweise
- ORD-Eintrag
- ord-ffc836c84ac84afe87e7418fbf9e4dc5
- Quelldatensatz
- uspto-grants-1998_07
- Patentnummer
- US05776652
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