Sodium Acetate → HCID 178525134, Verbindung

HRID 1351487Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1351487
Cl[C:2]1[N:7]=[N:6][C:5]([NH:8][CH2:9][CH:10]2[CH2:15][CH2:14][N:13]([C:16]([O:18][CH2:19][C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)=[O:17])[CH2:12][CH2:11]2)=[CH:4][CH:3]=1.C([O-])(=[O:28])C.[Na+]>C(O)(=O)C>[OH:28][C:2]1[N:7]=[N:6][C:5]([NH:8][CH2:9][CH:10]2[CH2:15][CH2:14][N:13]([C:16]([O:18][CH2:19][C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)=[O:17])[CH2:12][CH2:11]2)=[CH:4][CH:3]=1

Komponenten

4

Edukt 2

HCID 517045Sodium AcetateHCID 10155464HCID 10155464, Verbindung

Produkt 1

HCID 178525134HCID 178525134, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

Benzyl 4-{[(6-chloro-3-pyridazinyl)amino]methyl}-1-piperidinecarboxylate (EXAMPLE 22) (37 mg, 0.10 mmol) was dissolved in acetic acid (5 mL) with sodium acetate (82 mg, 1.00 mmol) and was heated to 100° C. for 18 h. The volatiles were removed under reduced pressure and the residue partitioned between sat. NaHCO3 and ethyl acetate. The organics were dried over Na2SO4, filtered and concentrated under reduced pressure, affording the title compound as a clear oil.

Aufarbeitung

  1. customThe volatiles were removed under reduced pressure
  2. customthe residue partitioned between sat. NaHCO3 and ethyl acetate
  3. dry with materialThe organics were dried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-43a2915f9ee94ba080ce53dba6c17cb8
Quelldatensatz
uspto-grants-2007_05
Patentnummer
US07217716B2

Notizen zur Reaktion

Wird geladen…