Hydrazine hydrate (1:1) → HCID 21187752, Verbindung

HRID 1383459Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1383459
[CH:1]([NH:14][CH:15]1[CH2:20][CH2:19][N:18]([CH2:21][CH2:22][N:23]2C(=O)C3C(=CC=CC=3)C2=O)[CH2:17][CH2:16]1)([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O.NN>C(O)C>[NH2:23][CH2:22][CH2:21][N:18]1[CH2:19][CH2:20][CH:15]([NH:14][CH:1]([C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=2)[C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)[CH2:16][CH2:17]1

Komponenten

4

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 21187763HCID 21187763, Verbindung

Produkt 1

HCID 21187752HCID 21187752, VerbindungAusbeute 7,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

The crude 2-{2-[4-(benzhydryl-amino)-piperidin-1-yl]-ethyl}-isoindole-1,3-dione (2.70 g) was dissolved in ethanol (5 ml), followed by the addition of hydrazine hydrate (large excess, 2-3 ml). The solution was stirred at room temperature overnight. The white solid was precipitated. The white solid was filtered off and washed with small amount of ethanol. The filtrates were combined and concentrated. The resulted residue was dissolved in toluene (100 ml). The solution was washed with water (3×15 ml) and dried over anhydrous Na2SO4. After evaporated the solvent, the crude product [1-(2-amino-ethyl)-piperidin-4-yl]-benzhydryl-amine was obtained (0.150 g, 7.9% yield).

Aufarbeitung

  1. customThe white solid was precipitated
  2. filtrationThe white solid was filtered off
  3. washwashed with small amount of ethanol
  4. concentrationconcentrated
  5. dissolutionThe resulted residue was dissolved in toluene (100 ml)
  6. washThe solution was washed with water (3×15 ml)
  7. dry with materialdried over anhydrous Na2SO4
  8. customAfter evaporated the solvent

Quellen und Nachweise

ORD-Eintrag
ord-93f5691102b34dcca72d6cd42ea24219
Quelldatensatz
uspto-grants-2001_07
Patentnummer
US06255323B1

Notizen zur Reaktion

Wird geladen…