Ethanol → HCID 20262414, Verbindung

HRID 371104Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 371104
[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 was 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-d9a01389ac6a4d459c90fdd5f5812f19
Quelldatensatz
uspto-grants-1985_07
Patentnummer
US04529727

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