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Ethanol → Bilastine

HRID 451237
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 451237
C([O:3][C:4](=[O:36])[C:5]([C:8]1[CH:13]=[CH:12][C:11]([CH2:14][CH2:15][N:16]2[CH2:21][CH2:20][CH:19]([C:22]3[N:26]([CH2:27][CH2:28][O:29][CH2:30][CH3:31])[C:25]4[CH:32]=[CH:33][CH:34]=[CH:35][C:24]=4[N:23]=3)[CH2:18][CH2:17]2)=[CH:10][CH:9]=1)([CH3:7])[CH3:6])C.[OH-].[Na+].C(O)C.O>C(O)CCC.C(OC(=O)C)C.C(O)(=O)C>[CH2:30]([O:29][CH2:28][CH2:27][N:26]1[C:25]2[CH:32]=[CH:33][CH:34]=[CH:35][C:24]=2[N:23]=[C:22]1[CH:19]1[CH2:20][CH2:21][N:16]([CH2:15][CH2:14][C:11]2[CH:10]=[CH:9][C:8]([C:5]([CH3:6])([CH3:7])[C:4]([OH:36])=[O:3])=[CH:13][CH:12]=2)[CH2:17][CH2:18]1)[CH3:31]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 4

HCID 702EthanolHCID 962WaterHCID 14798Sodium HydroxideHCID 66869688Ethyl 2-[4-(2-(4-(1-(2-ethoxyethyl)benzimidazole-2-yl)piperidine-1-yl)ethyl)phenyl]-2-methylpropanoate

Produkt 1

HCID 185460BilastineAusbeute 85 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 176
Acetic Acid
Lösungsmittel
HCID 2631-ButanolLösungsmittel
HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

In a reaction vessel, 2-[4-(2-{4-[1-(2-ethoxy-ethyl)-1H-benzoimidazol-2-yl]-piperidin-1-yl}-ethyl)-phenyl]-2-methyl-propionic acid ethylester (2.3 g) prepared in the Example 15, sodium hydroxide (0.6 g) and ethyl alcohol (13 mL) were introduced, and the mixture was reacted at 50-55□ for 3 hours. Distilled water (20 mL) was added thereto, and acetic acid was added to control the pH to 7. Ethylacetate (50 mL) was added thereto, and the mixture was stirred to separate layers. The separated organic layer was condensed under reduced pressure. And, butanol (9 mL) was added and dissolved by heating. And then, it was cooled to precipitate crystals, and the crystals were filtered under reduced pressure to obtain 2-[4-(2-{4-[1-(2-ethoxy-ethyl)-1H-benzoimidazol-2-yl]-piperidin-1-yl}-ethyl)-phenyl]-2-methyl-propionic acid (1.84 g, yield 85%, HPLC purity 99% or more).

Aufarbeitung

  1. additionwere introduced
  2. customthe mixture was reacted at 50-55□ for 3 hours
  3. customto separate layers
  4. customcondensed under reduced pressure
  5. dissolutiondissolved
  6. temperatureby heating
  7. temperatureAnd then, it was cooled
  8. customto precipitate crystals
  9. filtrationthe crystals were filtered under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-223de2c3fdb54e6a9ffb84ecc3fab67c
Quelldatensatz
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08487106B2

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