Sodium Hydroxide → 4-{2-[4-(3,3-Dimethyl-butyl)-piperazin-1-yl]-ethoxy}-3-methyl-benzoic Acid

HRID 220845Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 220845
C[O:2][C:3](=[O:26])[C:4]1[CH:9]=[CH:8][C:7]([O:10][CH2:11][CH2:12][N:13]2[CH2:18][CH2:17][N:16]([CH2:19][CH2:20][C:21]([CH3:24])([CH3:23])[CH3:22])[CH2:15][CH2:14]2)=[C:6]([CH3:25])[CH:5]=1.[OH-].[Na+]>O1CCOCC1>[CH3:22][C:21]([CH3:24])([CH3:23])[CH2:20][CH2:19][N:16]1[CH2:17][CH2:18][N:13]([CH2:12][CH2:11][O:10][C:7]2[CH:8]=[CH:9][C:4]([C:3]([OH:26])=[O:2])=[CH:5][C:6]=2[CH3:25])[CH2:14][CH2:15]1

Komponenten

4

Edukt 2

HCID 14798Sodium HydroxideHCID 575552114-{2-[4-(3,3-Dimethyl-butyl)-piperazin-1-yl]-ethoxy}-3-methyl-benzoic Acid Methyl Ester

Produkt 1

HCID 575552124-{2-[4-(3,3-Dimethyl-butyl)-piperazin-1-yl]-ethoxy}-3-methyl-benzoic AcidAusbeute 100 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

4-{2-[4-(3,3-Dimethyl-butyl)-piperazin-1-yl]-ethoxy}-3-methyl-benzoic acid methyl ester from Example E40.3 (42 mg, 0.12 mmol) was dissolved in dioxan (5 ml) and 1M NaOH (1 ml) was added. The mixture was heated at reflux for 2 h then solvents were concentrated in vacuo. The residue was dissolved in EtOAc, washed with saturated NaHCO3, water then brine, dried and concentrated in vacuo to yield the title compound (40 mg, 100%).

Aufarbeitung

  1. temperatureThe mixture was heated
  2. temperatureat reflux for 2 h
  3. concentrationsolvents were concentrated in vacuo
  4. dissolutionThe residue was dissolved in EtOAc
  5. washwashed with saturated NaHCO3, water
  6. dry with materialbrine, dried
  7. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-5bbdb2fd072b44be97f61975105033dd
Quelldatensatz
uspto-grants-2012_06
Patentnummer
US08202858B2

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