Sodium Hydroxide → (1-(2-hydroxyethyl)-1H-benzimidazol-2-yl)(piperidin-4-yl)amine

HRID 323511

Reaktionsgleichung

Reaktionsgleichung von HRID 323511
[OH:1][CH2:2][CH2:3][N:4]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[N:6]=[C:5]1[NH:13][CH:14]1[CH2:19][CH2:18][N:17](C(OCC)=O)[CH2:16][CH2:15]1.[OH-].[Na+]>C(O)(C)C.O>[OH:1][CH2:2][CH2:3][N:4]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[N:6]=[C:5]1[NH:13][CH:14]1[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]1

Komponenten

5

Edukt 2

HCID 14798Sodium HydroxideHCID 22009172(1-(2-hydroxyethyl)-1H-benzimidazol-2-yl)(1-(ethoxycarbonyl)piperidin-4-yl)amine

Produkt 1

HCID 22009128(1-(2-hydroxyethyl)-1H-benzimidazol-2-yl)(piperidin-4-yl)amine

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittel2×HCID 3776IsopropanolLösungsmittel

Versuchsvorschrift

Combine (1-(2-hydroxyethyl)-1H-benzimidazol-2-yl)(1-(ethoxycarbonyl)piperidin-4-yl)amine (5.0 mmol) and sodium hydroxide (2.0 g) in isopropanol (20 mL) and water (0.1 mL). Heat to reflux. After 36 hours, cool and evaporate the reaction mixture in vacuo to give a residue. Combine the residue and water. Extract the diluted residue three times with ethyl acetate. Combine the organic layers and extract with brine, dry over Na2SO4, filter, and evaporate in vacuo to give the title compound.

Aufarbeitung

  1. temperatureHeat to reflux
  2. temperaturecool
  3. customevaporate the reaction mixture in vacuo
  4. customto give a residue
  5. extractionExtract the diluted residue three times with ethyl acetate
  6. extractionextract with brine
  7. dry with materialdry over Na2SO4
  8. filtrationfilter
  9. customevaporate in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-97b2eacca48f4fa5a7262a1836bb0cc0
Quelldatensatz
uspto-grants-2001_04
Patentnummer
US06211199B1

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