Hydrochloric Acid → 4-(4-Methylpiperazin-1-yl)benzoic acid

HRID 1177935

Reaktionsgleichung

Reaktionsgleichung von HRID 1177935
[Li+].[OH-].C[O:4][C:5](=[O:19])[C:6]1[CH:11]=[CH:10][C:9]([N:12]2[CH2:17][CH2:16][N:15]([CH3:18])[CH2:14][CH2:13]2)=[CH:8][CH:7]=1.O.Cl>C1COCC1.O>[CH3:18][N:15]1[CH2:14][CH2:13][N:12]([C:9]2[CH:10]=[CH:11][C:6]([C:5]([OH:19])=[O:4])=[CH:7][CH:8]=2)[CH2:17][CH2:16]1

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 3939Lithium HydroxideHCID 1472668Methyl 4-(4-methylpiperazin-1-yl)benzoate

Produkt 1

HCID 7365324-(4-Methylpiperazin-1-yl)benzoic acidAusbeute 85,13 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 21881883Oxolane--water (1/1)Lösungsmittel

Versuchsvorschrift

LiOH (67 mg, 1.6 mmol) was added to a stirred solution 4-(4-methyl-piperazin-1-yl)-benzoic acid methyl ester (124 mg, 0.73 mmol) in THF:H2O (1:1, 4 mL), and the resulting mixture was stirred at room temperature overnight. The reaction mixture was concentrated under reduced pressure to get the residue. Cold water was then added and acidified it with 10% aqueous HCl and concentrated under reduced pressure to afford 116 mg (85.13% yield) of 4-(4-methyl-piperazin-1-yl)-benzoic acid. 1H NMR (DMSO-D2O): δ 7.8 (d, 2H), 7.0 (d, 2H), 3.4 (s, 4H), 2.8 (s, 4H), 2.4 (s, 3H).

Aufarbeitung

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customto get the residue
  3. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-e3ae7b1d8a90423cacf494b73e07d6df
Quelldatensatz
uspto-grants-2010_11
Patentnummer
US07842696B2

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