Water → 3-(4-(4-Methylpiperazin-1-yl)phenyl)butanamide

HRID 2176917Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2176917
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([C:8]2[CH:13]=[CH:12][C:11]([CH:14]([CH3:18])[CH2:15][C:16]#[N:17])=[CH:10][CH:9]=2)[CH2:4][CH2:3]1.[OH2:19]>C(=O)(O)[O-].[Na+]>[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([C:8]2[CH:13]=[CH:12][C:11]([CH:14]([CH3:18])[CH2:15][C:16]([NH2:17])=[O:19])=[CH:10][CH:9]=2)[CH2:4][CH2:3]1

Komponenten

4

Edukt 2

HCID 962WaterHCID 673833103-(4-(4-Methylpiperazin-1-yl)phenyl)butanenitrile

Produkt 1

HCID 673827633-(4-(4-Methylpiperazin-1-yl)phenyl)butanamideAusbeute 74 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 516892Sodium BicarbonateLösungsmittel

Reaktionsbedingungen

Temperatur
90 °C

Versuchsvorschrift

A suspension of 3-(4-(4-methylpiperazin-1-yl)phenyl)butanenitrile (450 mg, 1.85 mmol) and poly phosphoric acid (4.5 g) was heated at 90° C. for 3 h. The reaction mixture was cooled to room temperature, diluted with cold water and basified with saturated sodium bicarbonate solution. The aqueous layer was extracted with DCM, washed with water and brine solution. The organic layer was dried over sodium sulfate, filtered and concentrated in vacuo to afford 360 mg (74%) of 3-(4-(4-methylpiperazin-1-yl)phenyl)butanamide as light yellow color solid.

Aufarbeitung

  1. temperatureThe reaction mixture was cooled to room temperature
  2. extractionThe aqueous layer was extracted with DCM
  3. washwashed with water and brine solution
  4. dry with materialThe organic layer was dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-5b51626475174093a2302519680d8ffa
Quelldatensatz
uspto-grants-2015_06
Patentnummer
US09067888B2

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