Sodium Hydroxide → 3,4,5,6,7,8-Hexahydro-3-[2-(4-(2-methoxyphenyl)-1-piperazinyl)ethyl]pyrido[4',3'; 4,5]thieno[2,3-d]pyrimidin-4-one

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Reaktionsgleichung

C([N:4]1[CH2:33][CH2:32][C:7]2[C:8]3[C:13](=[O:14])[N:12]([CH2:15][CH2:16][N:17]4[CH2:22][CH2:21][N:20]([C:23]5[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=5[O:29][CH3:30])[CH2:19][CH2:18]4)[CH:11]=[N:10][C:9]=3[S:31][C:6]=2[CH2:5]1)(=O)C.[OH-].[Na+]>Cl>[CH3:30][O:29][C:24]1[CH:25]=[CH:26][CH:27]=[CH:28][C:23]=1[N:20]1[CH2:21][CH2:22][N:17]([CH2:16][CH2:15][N:12]2[C:13](=[O:14])[C:8]3[C:7]4[CH2:32][CH2:33][NH:4][CH2:5][C:6]=4[S:31][C:9]=3[N:10]=[CH:11]2)[CH2:18][CH2:19]1

Komponenten

Reaktionsbedingungen

Temperatur: 100 °C

Versuchsvorschrift

4.0 g (8.6 mmol) of 3,4,5,6,7,8-hexahydro-7-acetyl-3-[2-(4-(2-methoxyphenyl)piperazin-1-yl)ethyl]pyrido[4′,3′:4,5]thieno-[2,3-d]pyrimidin-4-one were dissolved in 80 ml of 10% strength hydrochloric acid and this solution was stirred at a bath temperature of 100° C. for 2 h. After that, the mixture was poured onto ice water and this mixture was rendered alkaline with conc. sodium hydroxide solution and extracted twice with methylene chloride. The combined organic phases were dried and evaporated. This resulted in the isolation of 3.7 g of crude product which was then recrystallized from 50 ml of isopropanol. 2.4 g (66%) of product having a m.p. of 168-170° C. were obtained.

Aufarbeitung

additionAfter that, the mixture was poured onto ice water
extractionextracted twice with methylene chloride
customThe combined organic phases were dried
customevaporated

Quellen und Nachweise

ORD-Eintrag: ord-d729167733764256bd2229a1f8d213eb
Quelldatensatz: uspto-grants-2002_05
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US06387912B1

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