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Water → HCID 19992337, Verbindung

HRID 345486
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 345486
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:16]2[CH:21]=[CH:20][C:19]([F:22])=[CH:18][CH:17]=2)([CH:10]2[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]2)[OH:9])=[CH:4][CH:3]=1.Cl[CH2:24][CH2:25][C:26]([N:28]([CH3:35])[C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)=[O:27].C(=O)([O-])[O-].[Na+].[Na+].O>CN(C)C=O.[I-].[K+]>[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:16]2[CH:17]=[CH:18][C:19]([F:22])=[CH:20][CH:21]=2)([OH:9])[CH:10]2[CH2:11][CH2:12][N:13]([CH2:24][CH2:25][C:26]([N:28]([CH3:35])[C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=3)=[O:27])[CH2:14][CH2:15]2)=[CH:4][CH:3]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 962WaterHCID 10340Sodium CarbonateHCID 33143863-chloro-N-methyl-N-phenylpropanamideHCID 11208889Bis(4-fluorophenyl)(piperidin-4-yl)methanol

Produkt 1

HCID 19992337HCID 19992337, VerbindungAusbeute 72 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 4875
Potassium Iodide
Katalysator
HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A mixture of 10.0 g (0.033 mole) of α,α-bis(4-fluorophenyl)-4-piperidine-methanol, 6.5 g (0.033 mole) of 3-chloro-N-methyl-N-phenylpropanamide, 14.0 g (0.132 mole) of anhydrous sodium carbonate and 0.3 g (0.002 mole) of potassium iodide in 100 ml of N,N-dimethylformamide was heated on a steam bath for 16 h. The mixture was poured into 2 L of water and extracted three times with 500 mL portions of ethyl acetate. The ethyl acetate fractions were combined, washed with water and brine, dried (MgSO4) and concentrated under reduced pressure to give a yellow glass. The glass was purified by column chromatography using 250 g of silica gel on a 65 cm×4 column, eluted with ethyl acetate. The fractions containing the desired product were combined and concentrated under reduced pressure to yield 11.0 g (72%) of a white solid. A portion of this solid was recrystallized from ethyl ether to give a white solid, mp 73°-75° C.

Aufarbeitung

  1. temperaturewas heated on a steam bath for 16 h
  2. extractionextracted three times with 500 mL portions of ethyl acetate
  3. washwashed with water and brine
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated under reduced pressure
  6. customto give a yellow glass
  7. customThe glass was purified by column chromatography
  8. washeluted with ethyl acetate
  9. additionThe fractions containing the desired product
  10. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-5b1d2dd8f508468f9e5aae9150e5daac
Quelldatensatz
uspto-grants-1991_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05057524

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