Piperidin-4-ol → HCID 178501992, Verbindung

HRID 47029Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 47029
Cl[C:2]1[N:7]=[C:6]([NH:8][C:9]([O:11][CH3:12])=[O:10])[N+:5]([O-:13])=[C:4]([NH:14][C:15]([O:17][CH3:18])=[O:16])[CH:3]=1.[OH:19][CH:20]1[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]1>C(Cl)Cl>[OH:19][CH:20]1[CH2:25][CH2:24][N:23]([C:2]2[N:7]=[C:6]([NH:8][C:9]([O:11][CH3:12])=[O:10])[N+:5]([O-:13])=[C:4]([NH:14][C:15]([O:17][CH3:18])=[O:16])[CH:3]=2)[CH2:22][CH2:21]1

Komponenten

4

Edukt 2

HCID 79341Piperidin-4-olHCID 178501976HCID 178501976, Verbindung

Produkt 1

HCID 178501992HCID 178501992, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A suspension of 2.5 g. of dimethyl 6-chloro-2,4-pyrimidine-dicarbamate-3-oxide in 100 ml. of methylene chloride is treated with 10 g. of 4-hydroxy-piperidine and stirred at room temperature under an argon atmosphere for 70 hours. The separated precipitate is filtered off and recrystallized from a mixture of methylene chloride and methanol, there being obtained pure dimethyl racemic-6-(4-hydroxy-1-piperidinyl)-2,4-pyrimidine-dicarbamate-3-oxide, having a melting point of 265°-266° C.

Aufarbeitung

  1. additionA suspension of 2.5 g
  2. filtrationThe separated precipitate is filtered off
  3. customrecrystallized from a mixture of methylene chloride and methanol, there

Quellen und Nachweise

ORD-Eintrag
ord-953fd860b1c84852b29f514e63241d88
Quelldatensatz
uspto-grants-1979_11
Patentnummer
US04176119

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