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Iodine → alpha,alpha-Bis(4-fluorophenyl)-1-(phenylmethyl)-4-piperidinemethanol

HRID 1193629
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1193629
[Mg].II.Br[C:5]1[CH:10]=[CH:9][C:8]([F:11])=[CH:7][CH:6]=1.Cl.C(O[C:16]([CH:18]1[CH2:23][CH2:22][N:21]([CH2:24][C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[CH2:20][CH2:19]1)=[O:17])C.[Cl-].[NH4+]>O1CCCC1>[F:11][C:8]1[CH:9]=[CH:10][C:5]([C:16]([C:5]2[CH:10]=[CH:9][C:8]([F:11])=[CH:7][CH:6]=2)([CH:18]2[CH2:19][CH2:20][N:21]([CH2:24][C:25]3[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=3)[CH2:22][CH2:23]2)[OH:17])=[CH:6][CH:7]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 5

HCID 807IodineHCID 99931-Bromo-4-fluorobenzeneHCID 25517Ammonium ChlorideHCID 5462224MagnesiumHCID 700922841-(Phenylmethyl)-4-piperidinecarboxylic acid ethyl ester hydrochloride

Produkt 1

HCID 13519964alpha,alpha-Bis(4-fluorophenyl)-1-(phenylmethyl)-4-piperidinemethanol
Ausbeute 51 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel3×

Versuchsvorschrift

To a 6.08 g (0.25 mole) of magnesium turnings and an iodine crystal in 600 ml of dry tetrahydrofuran and under an atmosphere of nitrogen was added, dropwise, a solution of p-bromofluorobenzene in 125 ml of tetrahydrofuran. The temperature of the reaction was kept below 10° C. by cooling in an ice-methanol bath. The mixture was stirred at room temperature for 1.5 hours. A solution of 24.7 g (0.10 mole) of 1-(phenylmethyl)-4-piperidinecarboxylic acid ethyl ester hydrochloride in tetrahydrofuran was added, and the mixture was stirred at room temperature for 17 hours. The reaction was poured into an icy, aqueous solution of ammonium chloride, and the resulting solution was extracted with methylene chloride. The methylene chloride solution was extracted with dilute sodium hydroxide and was dried over magnesium sulfate. The solvent was removed in vacuo to give an oil. This was crystallized from ether-hexane to give 19.87 g (51%) of the title compound, m.p. 113°-115° C.

Aufarbeitung

  1. customwas kept below 10° C.
  2. temperatureby cooling in an ice-methanol bath
  3. stirringthe mixture was stirred at room temperature for 17 hours
  4. extractionthe resulting solution was extracted with methylene chloride
  5. extractionThe methylene chloride solution was extracted with dilute sodium hydroxide
  6. dry with materialwas dried over magnesium sulfate
  7. customThe solvent was removed in vacuo
  8. customto give an oil
  9. customThis was crystallized from ether-hexane

Quellen und Nachweise

ORD-Eintrag
ord-0e74f6bea69e44e9b473a7cb314e57af
Quelldatensatz
uspto-grants-1989_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04810713

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