4-Chloro-6-hydrazinylpyrimidine → 4-Hydrazino-6-[4-(2-methoxyethyl)piperazin-1-yl]pyrimidine

HRID 242252

Reaktionsgleichung

Reaktionsgleichung von HRID 242252
Cl[C:2]1[CH:7]=[C:6]([NH:8][NH2:9])[N:5]=[CH:4][N:3]=1.[CH3:10][O:11][CH2:12][CH2:13][N:14]1[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]1>O>[NH:8]([C:6]1[CH:7]=[C:2]([N:17]2[CH2:18][CH2:19][N:14]([CH2:13][CH2:12][O:11][CH3:10])[CH2:15][CH2:16]2)[N:3]=[CH:4][N:5]=1)[NH2:9]

Komponenten

4

Edukt 2

HCID 2472224-Chloro-6-hydrazinylpyrimidineHCID 27346381-(2-Methoxyethyl)piperazine2×

Produkt 1

HCID 596036074-Hydrazino-6-[4-(2-methoxyethyl)piperazin-1-yl]pyrimidine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

A mixture of 1.0 g (6.9 mmol) of the compound from Example 7A and 1.1 g (7.6 mmol) 1-(2-methoxyethyl)piperazine in 10 ml water is stirred at 100° C. for 2 h. A further 0.9 g (6.2 mmol) 1-(2-methoxyethyl)piperazine is added and the reaction mixture is stirred further at 100° C. for 16 h. After concentration in vacuo, the residue is stirred in acetonitrile. The solid which has precipitated out is filtered off, washed first with ethanol and then with diethyl ether and dried in vacuo.

Aufarbeitung

  1. stirringthe reaction mixture is stirred further at 100° C. for 16 h
  2. concentrationAfter concentration in vacuo
  3. stirringthe residue is stirred in acetonitrile
  4. customThe solid which has precipitated out
  5. filtrationis filtered off
  6. washwashed first with ethanol
  7. dry with materialwith diethyl ether and dried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-e264a4d9c3c84af5924e926533b54e99
Quelldatensatz
uspto-grants-2014_02
Patentnummer
US08653111B2

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