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 1619445노트

반응식

HRID 1619445 반응식
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

참가 물질

3

반응물 1

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

생성물 1

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

시약·촉매·용매 1

HCID 180Acetone용매

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온도
27 °C

실험 절차

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

후처리

  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

출처 및 근거

ORD 기록
ord-985647bc66194a8db781db9ba6cf052c
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08772302B2

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