4-(4-(2,2-Dimethyl-1,3-dioxan-5-yl)phenoxy)-5-methyl-6-(1-(pyrimidin-2-yl)piperidin-4-yloxy)pyrimidine → 2-(4-(5-Methyl-6-(1-(pyrimidin-2-yl)piperidin-4-yloxy)pyrimidin-4-yloxy)phenyl)propane-1,3-diol

HRID 1619445Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1619445
CC1(C)[O:7][CH2:6][CH:5]([C:8]2[CH:34]=[CH:33][C:11]([O:12][C:13]3[C:18]([CH3:19])=[C:17]([O:20][CH:21]4[CH2:26][CH2:25][N:24]([C:27]5[N:32]=[CH:31][CH:30]=[CH:29][N:28]=5)[CH2:23][CH2:22]4)[N:16]=[CH:15][N:14]=3)=[CH:10][CH:9]=2)[CH2:4][O:3]1>CC(C)=O>[CH3:19][C:18]1[C:13]([O:12][C:11]2[CH:33]=[CH:34][C:8]([CH:5]([CH2:6][OH:7])[CH2:4][OH:3])=[CH:9][CH:10]=2)=[N:14][CH:15]=[N:16][C:17]=1[O:20][CH:21]1[CH2:26][CH2:25][N:24]([C:27]2[N:28]=[CH:29][CH:30]=[CH:31][N:32]=2)[CH2:23][CH2:22]1

Komponenten

3

Reaktionsbedingungen

Temperatur
27 °C

Versuchsvorschrift

To a solution of 4-(4-(2,2-dimethyl-1,3-dioxan-5-yl)phenoxy)-5-methyl-6-(1-(pyrimidin-2-yl)piperidin-4-yloxy)pyrimidine (1.5 gm, 0.0031 moles) in acetone (20 ml) conc. HCl (2 ml) was added portion-wise and the reaction mixture was stirred for 3 hours at 27° C. The reaction mixture was concentrated and the residue was dissolved in ethyl acetate. The organic extract was successively washed with water & brine, dried over sodium sulfate and evaporated under reduced pressure to yield 700 mg product as white solid

Aufarbeitung

  1. concentrationThe reaction mixture was concentrated
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. extractionThe organic extract
  4. washwas successively washed with water & brine
  5. dry with materialdried over sodium sulfate
  6. customevaporated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-985647bc66194a8db781db9ba6cf052c
Quelldatensatz
uspto-grants-2014_07
Patentnummer
US08772302B2

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