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Ethanol → Bilastine

HRID 451236
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 451236
C[O:2][C:3](=[O:35])[C:4]([C:7]1[CH:12]=[CH:11][C:10]([CH2:13][CH2:14][N:15]2[CH2:20][CH2:19][CH:18]([C:21]3[N:25]([CH2:26][CH2:27][O:28][CH2:29][CH3:30])[C:24]4[CH:31]=[CH:32][CH:33]=[CH:34][C:23]=4[N:22]=3)[CH2:17][CH2:16]2)=[CH:9][CH:8]=1)([CH3:6])[CH3:5].[OH-].[Na+].C(O)C.O>C(O)CCC.C(OC(=O)C)C.C(O)(=O)C>[CH2:29]([O:28][CH2:27][CH2:26][N:25]1[C:24]2[CH:31]=[CH:32][CH:33]=[CH:34][C:23]=2[N:22]=[C:21]1[CH:18]1[CH2:19][CH2:20][N:15]([CH2:14][CH2:13][C:10]2[CH:9]=[CH:8][C:7]([C:4]([CH3:5])([CH3:6])[C:3]([OH:35])=[O:2])=[CH:12][CH:11]=2)[CH2:16][CH2:17]1)[CH3:30]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 4

HCID 702EthanolHCID 962WaterHCID 14798Sodium HydroxideHCID 45257628Bilastine Ester

Produkt 1

HCID 185460BilastineAusbeute 90 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 176Acetic AcidLösungsmittel
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 methylester (2.3 g) prepared in the Example 14, sodium hydroxide (0.6 g) and ethylalcohol (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 a layer. The separated organic layer was condensed under reduced pressure. And, butanol (9 mL) was added thereto, 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 (2.0 g, yield 90%, HPLC purity 99% or more).

Aufarbeitung

  1. additionwere introduced
  2. customthe mixture was reacted at 50-55□ for 3 hours
  3. customto separate a layer
  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-df4022744de849e6ae6130c32a81c108
Quelldatensatz
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08487106B2

Notizen zur Reaktion

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