Hydrochloric Acid → HCID 22144532, Verbindung

HRID 1824792Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1824792
[ClH:1].[NH:2]1[C:10]2[C:5](=[CH:6][C:7]([C:11]#[N:12])=[CH:8][CH:9]=2)[CH:4]=[N:3]1.Cl.C([O:16][CH2:17][CH3:18])C.[CH2:19]([O:21][C:22]([C:24]1[CH:25]=[C:26]2[C:30](=[CH:31][CH:32]=1)[NH:29][N:28]=[CH:27]2)=[NH:23])[CH3:20]>C(O)C>[ClH:1].[CH2:19]([O:21][C:22]([C:24]1[CH:25]=[C:26]2[C:30](=[CH:31][CH:32]=1)[NH:29][N:28]=[CH:27]2)=[NH:23])[CH3:20].[NH:2]1[C:10]2[C:5](=[CH:6][C:7]([C:11]3[O:21][C:22]4[CH:18]=[C:17]([OH:16])[CH:31]=[CH:32][C:24]=4[N:12]=3)=[CH:8][CH:9]=2)[CH:4]=[N:3]1

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 22144493HCID 22144493, VerbindungHCID 69438029HCID 69438029, Verbindung

Produkt 2

HCID 22144532HCID 22144532, VerbindungHCID 69439754HCID 69439754, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

1H-Indazole-5-carbonitrile hydrochloride (1.5 g) was suspended in ethanol (15 mL) at 0° C. The mixture was saturated with hydrogen chloride while the temperature was raised to room temperature. The reaction was then left overnight. Diethylether was added and the resulting precipitate, 1H-indazole-5-carboximidic acid ethyl ester.2HCl (1.39 g), was collected and dried in under high vacuum. According to synthetic method B except that pyridine (540 ?L) was added, from 4-amino-benzene-1,3-diol hydrochloride (0.36 mg) and 1H-indazole-5-carboximidic acid ethyl ester hydrochloride (0.71 g) was obtained the title compound (0.34 mg) as an off-white solid. The work-up of the reaction was modified as follows: After completion of the reaction, the mixture was diluted with ether and water, and filtered. The solids were washed with water and ether, and dried under high vacuum. MS: 252.4 (MH+); HPLC tR: 1.80 min.

Aufarbeitung

  1. custom2HCl (1.39 g), was collected
  2. customdried in under high vacuum
  3. additionwas added, from 4-amino-benzene-1,3-diol hydrochloride (0.36 mg)

Quellen und Nachweise

ORD-Eintrag
ord-836ab09b49b2446698ce988653caef7e
Quelldatensatz
uspto-grants-2006_05
Patentnummer
US07045539B2

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