Trifluoroacetic acid → HCID 90203539, Verbindung

HRID 1480273

Reaktionsgleichung

Reaktionsgleichung von HRID 1480273
[CH:1]1([C:4]2[C:5]([O:25][C@@H:26]([CH3:31])[C:27]([F:30])([F:29])[F:28])=[CH:6][C:7]([C:10]([NH:12][CH:13]([C:21]([CH3:24])([CH3:23])[CH3:22])[C:14]([O:16]C(C)(C)C)=[O:15])=[O:11])=[N:8][CH:9]=2)[CH2:3][CH2:2]1.FC(F)(F)C(O)=O>ClCCl>[CH:1]1([C:4]2[C:5]([O:25][C@@H:26]([CH3:31])[C:27]([F:30])([F:28])[F:29])=[CH:6][C:7]([C:10]([NH:12][CH:13]([C:21]([CH3:24])([CH3:23])[CH3:22])[C:14]([OH:16])=[O:15])=[O:11])=[N:8][CH:9]=2)[CH2:3][CH2:2]1

Komponenten

4

Edukt 2

HCID 6422Trifluoroacetic acidHCID 90214929tert-butyl 2-[[5-cyclopropyl-4-[(1S)-2,2,2-trifluoro-1-methyl-ethoxy]pyridine-2-carbonyl]amino]-3,3-dimethyl-butanoate

Produkt 1

HCID 90203539HCID 90203539, VerbindungAusbeute 105,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a solution of tert-butyl 2-[[5-cyclopropyl-4-[(1S)-2,2,2-trifluoro-1-methyl-ethoxy]pyridine-2-carbonyl]amino]-3,3-dimethyl-butanoate (example 199a, 0.485 g, 1.09 mmol) in dichloromethane (3 ml) was added trifluoroacetic acid (3.73 g, 2.52 ml, 32.8 mmol) and the reaction mixture was stirred at room temperature for 14 hours. Volatiles were removed in vacuo and the residue was dissolved in toluene followed by evaporation to dryness. The procedure was repeated twice to yield the title compound (446 mg) as a crude solid which was used without any purification. MS (ESI, m/z): 387.5 (M−H+).

Aufarbeitung

  1. customVolatiles were removed in vacuo
  2. dissolutionthe residue was dissolved in toluene
  3. customfollowed by evaporation to dryness

Quellen und Nachweise

ORD-Eintrag
ord-1c9d3879c3994f23a3ee7c7ba490eb15
Quelldatensatz
uspto-grants-2016_08
Patentnummer
US09409866B2

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