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Triethylamine → 2-[4-[3-Chloro-4-(hydroxymethyl)phenyl]-1-piperazinyl]-1-(2-benzofuranyl)-ethanone

HRID 462423
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 462423
[C:1]([C:4]1[O:5][C:6]2[CH:12]=[CH:11][CH:10]=[CH:9][C:7]=2[CH:8]=1)(=[O:3])[CH3:2].BrBr.C(=O)(O)[O-].[Na+].[Cl:20][C:21]1[CH:26]=[C:25]([N:27]2[CH2:32][CH2:31][NH:30][CH2:29][CH2:28]2)[CH:24]=[CH:23][C:22]=1[CH2:33][OH:34].C(N(CC)CC)C>CCOCC.CC(C)=O>[Cl:20][C:21]1[CH:26]=[C:25]([N:27]2[CH2:32][CH2:31][N:30]([CH2:2][C:1]([C:4]3[O:5][C:6]4[CH:12]=[CH:11][CH:10]=[CH:9][C:7]=4[CH:8]=3)=[O:3])[CH2:29][CH2:28]2)[CH:24]=[CH:23][C:22]=1[CH2:33][OH:34]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 5

HCID 8471TriethylamineHCID 154352-AcetylbenzofuranHCID 24408BromineHCID 516892Sodium BicarbonateHCID 134571012-Chloro-4-(1-piperazinyl)benzenemethanol

Produkt 1

HCID 134571502-[4-[3-Chloro-4-(hydroxymethyl)phenyl]-1-piperazinyl]-1-(2-benzofuranyl)-ethanone

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 180AcetoneLösungsmittelHCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

A solution of 2-acetylbenzofuran (3.2 g. 0.02) in ether (50 ml) was treated with bromine (3.2 g., 0.02 mole) portionwise at room temperature. The mixture rapidly decolorized to a light yellow solution that was poured into cold aqueous sodium bicarbonate. The layers were separated and the aqueous layer was extracted with ether. The combined ether extracts were dried (K2CO3) and the ether was removed in vacuo, keeping the mixture cold. The gummy, off-white solid was dissolved in acetone (50 ml) and quickly added to a solution of 2-chloro-4-(1-piperazinyl)benzenemethanol (4.0 g, 0.0176 mole) and triethylamine (2.0 g, 0.902 mole) in acetone (200 ml). The mixture was stirred at room temperature for one hour, then cooled in an ice bath. The solid was collected, washed with ether, and air dried. Recrystallization from acetone-ethanol gave 3.7 g (55%), mp 169°-172°.

Aufarbeitung

  1. customThe layers were separated
  2. extractionthe aqueous layer was extracted with ether
  3. dry with materialThe combined ether extracts were dried (K2CO3)
  4. customthe ether was removed in vacuo
  5. dissolutionThe gummy, off-white solid was dissolved in acetone (50 ml)
  6. temperaturecooled in an ice bath
  7. customThe solid was collected
  8. washwashed with ether, and air
  9. customdried
  10. customRecrystallization from acetone-ethanol
  11. customgave 3.7 g (55%), mp 169°-172°

Quellen und Nachweise

ORD-Eintrag
ord-4ad655b2ba1847409c22775831909eab
Quelldatensatz
uspto-grants-1985_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04515793

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