Trifluoroacetic acid → HCID 65439120, Verbindung

HRID 2041894Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2041894
[F:1][C:2]1[CH:3]=[C:4]([C:9]2([OH:20])[CH2:12][N:11](C(OC(C)(C)C)=O)[CH2:10]2)[CH:5]=[CH:6][C:7]=1[F:8].FC(F)(F)C(O)=O>ClCCl>[F:1][C:2]1[CH:3]=[C:4]([C:9]2([OH:20])[CH2:12][NH:11][CH2:10]2)[CH:5]=[CH:6][C:7]=1[F:8]

Komponenten

4

Edukt 2

HCID 6422Trifluoroacetic acidHCID 659188071,1-Dimethylethyl 3-(3,4-difluorophenyl)-3-hydroxy-1-azetidinecarboxylate

Produkt 1

HCID 65439120HCID 65439120, VerbindungAusbeute 75,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A mixture of tert-butyl 3-(3,4-difluorophenyl)-3-hydroxyazetidine-1-carboxylate (1.06 g, 3.72 mmol) and trifluoroacetic acid (3 ml) in dichloromethane (30 ml) was stirred at ambient temperature for 1.5 h. The solvent was evaporated and the crude product was purified on a Biotage Isolute SCX-3 SPE column (washed with methanol and eluted with methanol/triethylamine, 4:1) to give the title compound (0.52 g). MS m/z (rel. intensity, 70 eV) 185 (M+, 1), 156 (50), 141 (bp), 127 (58), 114 (90).

Aufarbeitung

  1. customThe solvent was evaporated
  2. customthe crude product was purified on a Biotage Isolute SCX-3 SPE column (washed with methanol and eluted with methanol/triethylamine, 4:1)

Quellen und Nachweise

ORD-Eintrag
ord-154574165eac406c87b3cc9c5dc9d2b6
Quelldatensatz
uspto-grants-2013_11
Patentnummer
US08586572B2

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