Hydrochloric Acid → Piperazine-1-carboxylic acid (7-methoxy-thiazolo[5,4-d]pyrimidin-2-yl)-amide hydrochloride

HRID 550810Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 550810
[ClH:1].C(OC([N:9]1[CH2:14][CH2:13][N:12]([C:15](=[O:28])[NH:16][C:17]2[S:18][C:19]3[N:20]=[CH:21][N:22]=[C:23]([O:26][CH3:27])[C:24]=3[N:25]=2)[CH2:11][CH2:10]1)=O)(C)(C)C>C(Cl)Cl>[ClH:1].[CH3:27][O:26][C:23]1[C:24]2[N:25]=[C:17]([NH:16][C:15]([N:12]3[CH2:11][CH2:10][NH:9][CH2:14][CH2:13]3)=[O:28])[S:18][C:19]=2[N:20]=[CH:21][N:22]=1

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 590119304-(7-Methoxy-thiazolo[5,4-d]pyrimidin-2-ylcarbamoyl)-piperazine-1-carboxylic acid tert-butyl ester

Produkt 1

HCID 86616506Piperazine-1-carboxylic acid (7-methoxy-thiazolo[5,4-d]pyrimidin-2-yl)-amide hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
25 °C

Versuchsvorschrift

Hydrogen chloride gas was bubbled through a solution of 4-(7-methoxy-thiazolo[5,4-d]pyrimidin-2-ylcarbamoyl)-piperazine-1-carboxylic acid tert-butyl ester (5.20 g, 13 mmol) in methylene chloride (70 mL) for 10 min at 0° C. A white precipitate formed. The resulting slurry was stirred at 25° C. for 2 h. At this time, the mixture was concentrated in vacuo and dried under high vacuum to afford piperazine-1-carboxylic acid (7-methoxy-thiazolo[5,4-d]pyrimidin-2-yl)-amide hydrochloride (4.61 g) as a white solid; LRMS for C11H14N6O2S (M+H)+ at m/z=295. This solid was used in the next step without further purification.

Aufarbeitung

  1. customA white precipitate formed
  2. concentrationAt this time, the mixture was concentrated in vacuo
  3. customdried under high vacuum

Quellen und Nachweise

ORD-Eintrag
ord-ff6a7e27a8fb403d85a3024830d7eaee
Quelldatensatz
uspto-grants-2011_05
Patentnummer
US07947692B2

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