Ethanol → HCID 20262414, Verbindung

HRID 464670Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 464670
[NH:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3]([CH:10]2[CH2:15][CH2:14][N:13]([CH2:16][CH2:17][C:18]3[C:23](=[O:24])[N:22]4[C:25]([CH3:28])=[CH:26][S:27][C:21]4=[N:20][C:19]=3[CH3:29])[CH2:12][CH2:11]2)=[CH:2]1.C(O)C.[P:33](=[O:37])([OH:36])([OH:35])[OH:34]>O>[P:33]([OH:37])([OH:36])([OH:35])=[O:34].[NH:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3]([CH:10]2[CH2:15][CH2:14][N:13]([CH2:16][CH2:17][C:18]3[C:23](=[O:24])[N:22]4[C:25]([CH3:28])=[CH:26][S:27][C:21]4=[N:20][C:19]=3[CH3:29])[CH2:12][CH2:11]2)=[CH:2]1

Komponenten

5

Edukt 3

HCID 702EthanolHCID 1004Phosphoric AcidHCID 30861076-(2-(4-(1H-Indol-3-yl)piperidin-1-yl)ethyl)-3,7-dimethyl-5H-thiazolo(3,2-a)pyrimidin-5-one

Produkt 1

HCID 20262414HCID 20262414, VerbindungAusbeute 80 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A stirred and warm suspension of 4 parts of 6-[2-[4-(1H-indol-3-yl)-1-piperidinyl]ethyl]-3,7-dimethyl-5H-thiazolo[3,2-a]pyrimidin-5-one in 80 parts of ethanol was acidified with phosphoric acid. 60 Parts of water were added and the whole as boiled. The undissolved material was filtered off and the filtrate was allowed to crystallize. The product was filtered off and dried, yielding 4.5 parts (80%) of 6-[2-[4-(1H-indol-3-yl)-1-piperidinyl]ethyl]-3,7-dimethyl-5H-thiazolo[3,2-a]pyrimidin-5-one phosphate (2:3) monohydrate; mp. 214.4° C. (compound 28).

Aufarbeitung

  1. temperaturewarm
  2. filtrationThe undissolved material was filtered off
  3. customto crystallize
  4. filtrationThe product was filtered off
  5. customdried

Quellen und Nachweise

ORD-Eintrag
ord-4cd6baa77fcb4b71a93da45fd49f0416
Quelldatensatz
uspto-grants-1985_10
Patentnummer
US04548938

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