Hydrochloric Acid → HCID 136082911, Verbindung

HRID 1788000Notizen

Reaktionsgleichung

C[O:2][C:3]1[CH:11]=[C:10]2[C:6]([C:7]([N:12]3[C:20](=[O:21])[C:19]4[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=4)[C:13]3=[O:22])=[N:8][NH:9]2)=[CH:5][CH:4]=1.Cl.N1C=CC=CC=1.Cl>C(OCC)(=O)C>[OH:2][C:3]1[CH:11]=[C:10]2[C:6]([C:7]([N:12]3[C:20](=[O:21])[C:19]4[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=4)[C:13]3=[O:22])=[N:8][NH:9]2)=[CH:5][CH:4]=1

Komponenten

Reaktionsbedingungen

Temperatur: 200 °C

Versuchsvorschrift

A mixture of 24.2 g (82.5 mmol) of 2-({6-methoxy}-1H-indazol-3-yl)-1H-isoindole-1,3(2H)-dione and 73.4 g (0.635 mol) of piridine hydrochloride was heated at 200° C. for 4 hours. The resulting brown solution was cooled to 140° C. and slowly poured in a well stirred mixture of 250 ml of 0.2 N HCl and 350 ml of ethyl acetate. The organic layer was separated and the aqueous layer was salted (45 g of NaCl) and extracted twice with 350 ml of ethyl acetate. Organic extracts were dried over sodium sulfate and concentrated under vacuum to small volume. The precipitate was filtered off and dried: 15.89 g of product as yellow solid were obtained. Yield=68.9%. mp=265-270° C. dec.

Aufarbeitung

temperatureThe resulting brown solution was cooled to 140° C.
additionslowly poured in a well
customThe organic layer was separated
extractionextracted twice with 350 ml of ethyl acetate
dry with materialOrganic extracts were dried over sodium sulfate
concentrationconcentrated under vacuum to small volume
filtrationThe precipitate was filtered off
customdried

Quellen und Nachweise

ORD-Eintrag: ord-f12aead606f24a7b964da767f75a6aec
Quelldatensatz: uspto-grants-2009_03
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US07511136B2

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