Dichloromethane → HCID 18980339, Verbindung

0.50 g (0.0013 mol) of 2-ethoxycarbonyl-4-(3,4-methylenedioxybenzyl)amino-6-chloroquinazoline was dissolved in a solvent mixture comprising 20 ml of methylene chloride and 20 ml of tetrahydrofuran. 2.6 ml of a 1.0M solution of diisobutylaluminum hydride in toluene was dropped into the solution prepared above at -78° C. under stirring. The obtained mixture was stirred at -78° C. for several hours, followed by the addition of 20 ml of methanol. The obtained mixture was distilled under a reduced pressure to remove the solvent. The residue was purified by silica gel column chromatography and recrystallized from ethyl acetate/n-hexane to give 0.23 g of the title compound as a pale-yellow crystal.

1. customprepared above at -78° C.
2. stirringThe obtained mixture was stirred at -78° C. for several hours
3. distillationThe obtained mixture was distilled under a reduced pressure
4. customto remove the solvent
5. customThe residue was purified by silica gel column chromatography
6. customrecrystallized from ethyl acetate/n-hexane

ORD-Eintrag

ord-b51894dc936346e9af7f3d0d48f7e1e9

Quelldatensatz

uspto-grants-1998_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05801180