Reaktionsgleichung
C(=[N:8][C:9]([CH2:19][CH3:20])([CH2:15][CH2:16][CH2:17][CH3:18])[C:10]([O:12][CH2:13][CH3:14])=[O:11])C1C=CC=CC=1.Cl>>[NH2:8][C:9]([CH2:19][CH3:20])([CH2:15][CH2:16][CH2:17][CH3:18])[C:10]([O:12][CH2:13][CH3:14])=[O:11]Komponenten
3
Reaktionsbedingungen
- Temperatur
- 10 °C
Versuchsvorschrift
A solution of the product from step (c) (1mole) in 1N aqu. HCl (1.2 moles) was stirred for 10 minutes at room temperature, then washed with toluene. The pH of the remaining aqueous phase was adjusted to 7 using 12.5% w/v sodium hydroxide, then cooled to 10° C., further basified to pH 12 and extracted with toluene. The extracts were combined, washed with brine, dried and evaporated in vacuo. The residue was distilled to give the desired product as an oil (70-80% yield).
Aufarbeitung
- washwashed with toluene
- extractionextracted with toluene
- washwashed with brine
- customdried
- customevaporated in vacuo
- distillationThe residue was distilled
Quellen und Nachweise
- ORD-Eintrag
- ord-f4b79fcdd4274acc9f776993d7dd934b
- Quelldatensatz
- uspto-grants-1999_01
- Patentnummer
- US05859240
Verknüpfte Notizen
Wird geladen…