Reaktionsgleichung
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[N:12][C:13]([C:15]2[C:24]3[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=3)[CH:18]=[CH:17][CH:16]=2)=O)OCC)=[CH:4][CH:3]=1.[C:25]1([NH:35][NH2:36])[C:34]2[C:29](=[CH:30][CH:31]=[CH:32][CH:33]=2)[CH:28]=[CH:27][CH:26]=1>C(Cl)(Cl)(Cl)Cl>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:12]=[C:13]([C:15]3[C:24]4[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=4)[CH:18]=[CH:17][CH:16]=3)[N:35]([C:25]3[C:34]4[C:29](=[CH:30][CH:31]=[CH:32][CH:33]=4)[CH:28]=[CH:27][CH:26]=3)[N:36]=2)=[CH:4][CH:3]=1Komponenten
4
Reaktionsbedingungen
- Temperatur
- 25 °C
Versuchsvorschrift
The compound obtained in step A) (1.0 g, 0.026 mol) and 1-naphthyl hydrazine (0.45 g, 0.028 mol) is dissolved in CCl4 (15 ml) and stirred for 10 hours at 25° C. under a nitrogen atmosphere. The reaction mixture is stirred for 12 hours and filtered to remove traces of insoluble particles. The CCl4 solution is then concentrated and a few drops of methanol are added to the residue, wherein a brownish solid is obtained (Yield=0.7 g (56%)).
Aufarbeitung
- stirringThe reaction mixture is stirred for 12 hours
- filtrationfiltered
- customto remove traces of insoluble particles
- concentrationThe CCl4 solution is then concentrated
- additiona few drops of methanol are added to the residue, wherein a brownish solid
- customis obtained (Yield=0.7 g (56%))
Quellen und Nachweise
- ORD-Eintrag
- ord-d7c2db3732134b1683088925a9ff0fc8
- Quelldatensatz
- uspto-grants-2015_08
- Patentnummer
- US09113536B2
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