Water → 3-Chloro-4-(4-methylpiperazin-1-yl)aniline

HRID 1446119

Reaktionsgleichung

Reaktionsgleichung von HRID 1446119
C(OC(=O)[NH:7][C:8]1[CH:13]=[CH:12][C:11]([N:14]2[CH2:19][CH2:18][N:17]([CH3:20])[CH2:16][CH2:15]2)=[C:10]([Cl:21])[CH:9]=1)(C)(C)C.O.C([O-])(O)=O.[Na+]>Cl.O1CCOCC1>[Cl:21][C:10]1[CH:9]=[C:8]([NH2:7])[CH:13]=[CH:12][C:11]=1[N:14]1[CH2:15][CH2:16][N:17]([CH3:20])[CH2:18][CH2:19]1

Komponenten

6

Edukt 3

HCID 962WaterHCID 516892Sodium BicarbonateHCID 66870439HCID 66870439, Verbindung

Produkt 1

HCID 8203433-Chloro-4-(4-methylpiperazin-1-yl)aniline

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 313Hydrochloric AcidLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

298 mg (0.92 mmol) of [3-chloro-4-(4-methyl-piperazin-1-yl)-phenyl]-carbamic acid tert-butyl ester (Example 65b) are dissolved in 5 ml of 4 N HCl in dioxane. The solution is stirred for 4 h at 50° C., and after this time water is added and the pH is adjusted to 8 with NaHCO3. The suspension is extracted with n-butanol. The organic phase is washed with water, dried over MgSO4 and evaporated to dryness to provide the title compound. Title compound: ES-MS: 226.2 (M+H)+; analytical HPLC: tret=3.09 minutes (Grad 2).

Aufarbeitung

  1. extractionThe suspension is extracted with n-butanol
  2. washThe organic phase is washed with water
  3. dry with materialdried over MgSO4
  4. customevaporated to dryness

Quellen und Nachweise

ORD-Eintrag
ord-8367b4a467d5473790936fe5a44be2f8
Quelldatensatz
uspto-grants-2010_02
Patentnummer
US07667039B2

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