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 1619445ノート

反応式

HRID 1619445 の反応式
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

参加物

3

反応物 1

HCID 675115354-(4-(2,2-Dimethyl-1,3-dioxan-5-yl)phenoxy)-5-methyl-6-(1-(pyrimidin-2-yl)piperidin-4-yloxy)pyrimidine

生成物 1

HCID 675119332-(4-(5-Methyl-6-(1-(pyrimidin-2-yl)piperidin-4-yloxy)pyrimidin-4-yloxy)phenyl)propane-1,3-diol収率 51.6%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

反応条件

温度
27 °C

実験手順

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

後処理

  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

出典と根拠

ORDレコード
ord-985647bc66194a8db781db9ba6cf052c
出典データセット
uspto-grants-2014_07
特許番号
US08772302B2

反応ノート

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