Trifluoroacetic acid → 4-[4-(4,5-Dihydrooxazol-2-yl)phenyl]piperazine

HRID 650928Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 650928
C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[CH:19]=[CH:18][C:17]([C:20]3[O:21][CH2:22][CH2:23][N:24]=3)=[CH:16][CH:15]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.FC(F)(F)C(O)=O>C1(C)C=CC=CC=1.CO.C(N(CC)CC)C>[O:21]1[CH2:22][CH2:23][N:24]=[C:20]1[C:17]1[CH:18]=[CH:19][C:14]([N:11]2[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]2)=[CH:15][CH:16]=1

Komponenten

6

Edukt 2

HCID 6422Trifluoroacetic acidHCID 18504842n-Tert-butoxycarbonyl-4-[4-(4,5-dihydrooxazol-2-yl)phenyl]piperazine

Produkt 1

HCID 185048344-[4-(4,5-Dihydrooxazol-2-yl)phenyl]piperazine

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 887MethanolLösungsmittelHCID 1140TolueneLösungsmittelHCID 8471TriethylamineLösungsmittel

Versuchsvorschrift

Compound 5A (826 mg; 2.49 mmol) in solution in toluene (20 ml) is treated, at room temperature, with trifluoroacetic acid (2.75 ml). After 1 h, the medium is evaporated to dryness and coevaporated 3 times with toluene. The product obtained is taken up in methanol (20 ml) and triethylamine (8 ml), stirred for 15 min at room temperature and finally evaporated to dryness. The solid obtained is purified by chromatography on a silica gel column eluted with a dichloro-methane/methanol/ammonium hydroxide mixture in the proportions 90/9/1 to give the intermediate 5B.

Aufarbeitung

  1. customthe medium is evaporated to dryness
  2. customThe product obtained
  3. customfinally evaporated to dryness
  4. customThe solid obtained
  5. customis purified by chromatography on a silica gel column
  6. washeluted with a dichloro-methane/methanol/ammonium hydroxide mixture in the proportions 90/9/1

Quellen und Nachweise

ORD-Eintrag
ord-a21c3b9c151343858ede89557582c309
Quelldatensatz
uspto-grants-2001_08
Patentnummer
US06277853B1

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