Trifluoroacetic acid → N-(2-[(2,3-Difluorobenzyl)thio]-6-{[(1R,2S)-2,3-dihydroxy-1-methylpropyl]oxy}pyrimidin-4-yl)morpholine-4-sulfonamide

HRID 1024934Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1024934
[F:1][C:2]1[C:35]([F:36])=[CH:34][CH:33]=[CH:32][C:3]=1[CH2:4][S:5][C:6]1[N:11]=[C:10]([NH:12][S:13]([N:16]2[CH2:21][CH2:20][O:19][CH2:18][CH2:17]2)(=[O:15])=[O:14])[CH:9]=[C:8]([O:22][C@@H:23]([C@@H:25]2[CH2:29][O:28]C(C)(C)[O:26]2)[CH3:24])[N:7]=1.C(O)(C(F)(F)F)=O>CO>[F:1][C:2]1[C:35]([F:36])=[CH:34][CH:33]=[CH:32][C:3]=1[CH2:4][S:5][C:6]1[N:11]=[C:10]([NH:12][S:13]([N:16]2[CH2:21][CH2:20][O:19][CH2:18][CH2:17]2)(=[O:15])=[O:14])[CH:9]=[C:8]([O:22][C@H:23]([CH3:24])[C@@H:25]([OH:26])[CH2:29][OH:28])[N:7]=1

Komponenten

4

Versuchsvorschrift

To a solution of N-(2-[(2,3-difluorobenzyl)thio]-6-{(1R)-1-[(4S)-2,2-dimethyl-1,3-dioxolan-4-yl]ethoxy}pyrimidin-4-yl)morpholine-4-sulfonamide (0.20 g) in MeOH (2 ml) was added TFA (0.4 ml) and the reaction was stirred at room temperature for 20 h. The mixture was evaporated, suspended in saturated sodium carbonate solution and then re-acidified to pH5 with glacial acetic acid with stirring. The resulting solid was collected, washed with H2O and dried to give the title compound as a white solid. Yield 0.15 g.

Aufarbeitung

  1. customThe mixture was evaporated
  2. stirringre-acidified to pH5 with glacial acetic acid with stirring
  3. customThe resulting solid was collected
  4. washwashed with H2O
  5. customdried

Quellen und Nachweise

ORD-Eintrag
ord-e7a2584945504fe8a4566a1bf21607ba
Quelldatensatz
uspto-grants-2014_05
Patentnummer
US08722883B2

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