Triethylamine → HCID 13478095, Verbindung

HRID 280095

Reaktionsgleichung

Cl[C:2]1[N:11]=[CH:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.[F:12][C:13]1[CH:18]=[CH:17][C:16]([C:19]2([CH2:24][CH2:25][CH2:26][N:27]3[CH2:32][CH2:31][NH:30][CH2:29][CH2:28]3)OCC[O:20]2)=[CH:15][CH:14]=1.C(N(CC)CC)C>C(O)(C)C>[N:3]1[C:4]2[C:9](=[CH:8][CH:7]=[CH:6][CH:5]=2)[CH:10]=[N:11][C:2]=1[N:30]1[CH2:29][CH2:28][N:27]([CH2:26][CH2:25][CH2:24][C:19]([C:16]2[CH:15]=[CH:14][C:13]([F:12])=[CH:18][CH:17]=2)=[O:20])[CH2:32][CH2:31]1

Komponenten

Reaktionsbedingungen

Temperatur: 80 °C

Versuchsvorschrift

2.25 g 2-Chloroquinazoline, 4.2 g 1-(3-[2-(4-fluorophenyl)-1,3-dioxolan-2-yl]-propyl)piperazine and 2 ml triethylamine in 8 ml isopropanol are stirred and heated 21/2 hours at 80° C. The solvent is then evaporated in vacuo and the residue is taken up in hexane. The hexane solution is treated with charcoal, filtered and concentrated whereby the ketal of the title compound crystallizes out. The resulting precipitate is dissolved in 40 ml aqueous 1N hydrochloric acid. After 1 hour the acidic solution is made alkaline with aqueous ammonia. The resulting precipitate is filtered off and recrystallized from ethyl acetate to give the title compound, m.p. 129°-131° C.

Aufarbeitung

customThe solvent is then evaporated in vacuo
additionThe hexane solution is treated with charcoal
filtrationfiltered
concentrationconcentrated whereby the ketal of the title compound
customcrystallizes out
dissolutionThe resulting precipitate is dissolved in 40 ml aqueous 1N hydrochloric acid
filtrationThe resulting precipitate is filtered off
customrecrystallized from ethyl acetate

Quellen und Nachweise

ORD-Eintrag: ord-08454f3608f04742afd7aee3d64b3985
Quelldatensatz: uspto-grants-1986_05
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US04588725

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