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HCID 70574680, Verbindung → 2-[(4-methoxyphenyl)methyl]pyrrolidine

HRID 1278037
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1278037
C(OC([C:8](=[C:17]1[CH2:21][CH2:20][CH2:19][NH:18]1)[C:9]1[CH:14]=[CH:13][C:12]([O:15][CH3:16])=[CH:11][CH:10]=1)=O)(C)(C)C>FC(F)(F)C(O)=O>[CH3:16][O:15][C:12]1[CH:11]=[CH:10][C:9]([CH2:8][CH:17]2[CH2:21][CH2:20][CH2:19][NH:18]2)=[CH:14][CH:13]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

3

Edukt 1

HCID 70574680HCID 70574680, Verbindung

Produkt 1

HCID 49955292-[(4-methoxyphenyl)methyl]pyrrolidine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6422Trifluoroacetic acidLösungsmittel

Versuchsvorschrift

Add 80 ml of trifluoroacetic acid to 15 g of the title compound of Example 17 with ice cooling, and stir the produced reaction mixture for 2 hours at room temperature. Distil off the acid under a vacuum. Dissolve the resulting residue in 250 ml of diethyl ether and wash the thus-prepared solution with almost saturated cold sodium carbonate solution (150 ml) and saturated sodium chloride solution. Dry the washed solution over sodium sulfate and distil off the ether before dissolving the residue in 300 ml of ethanol and reducing it with Raney nickel/hydrogen. Concentrate the reduced solution to an oil and distil the oil under a vacuum to obtain 7.5 g (76% of theory) of the title compound (b.p. 88° to 90° at 0.008 mm of Hg).

Aufarbeitung

  1. customthe produced reaction mixture for 2 hours at room temperature
  2. customDistil off the acid under a vacuum
  3. dissolutionDissolve the resulting residue in 250 ml of diethyl ether
  4. washwash the thus-prepared solution with almost saturated cold sodium carbonate solution (150 ml) and saturated sodium chloride solution
  5. dry with materialDry the washed solution over sodium sulfate
  6. customdistil off the ether
  7. dissolutionbefore dissolving the residue in 300 ml of ethanol
  8. concentrationConcentrate the reduced solution to an oil
  9. customdistil the oil under a vacuum

Quellen und Nachweise

ORD-Eintrag
ord-61357ace7ab640d18f12334116565d3e
Quelldatensatz
uspto-grants-1981_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04279918

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