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Ethyl Acetate → HCID 178440648、化合物

HRID 2048572
ノート
印刷プレビュー

反応式

HRID 2048572 の反応式
[Si]([O:8][CH:9]1[CH2:14][CH2:13][CH:12]([NH:15][C:16]2[NH:20][N:19]=[CH:18][CH:17]=2)[CH2:11][CH2:10]1)(C(C)(C)C)(C)C.N12CCCN=C1CCCCC2.[C:32]([C:34]1[CH:39]=[CH:38][CH:37]=[CH:36][C:35]=1[C:40]1[N:45]=[CH:44][C:43]([CH2:46][CH:47]([C:52](=O)[CH2:53][CH2:54][CH2:55][CH3:56])[C:48](OC)=[O:49])=[CH:42][CH:41]=1)#[N:33].C(OCC)(=O)C>CCN(C1C=CC=CC=1)CC.O>[CH2:53]([C:52]1[N:20]2[N:19]=[CH:18][CH:17]=[C:16]2[N:15]([C@H:12]2[CH2:11][CH2:10][C@H:9]([OH:8])[CH2:14][CH2:13]2)[C:48](=[O:49])[C:47]=1[CH2:46][C:43]1[CH:42]=[CH:41][C:40]([C:35]2[CH:36]=[CH:37][CH:38]=[CH:39][C:34]=2[C:32]#[N:33])=[N:45][CH:44]=1)[CH2:54][CH2:55][CH3:56]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 8857Ethyl AcetateHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 67008908Methyl 2-{[6-(2-cyanophenyl)pyridin-3-yl]methyl}-3-oxoheptanoateHCID 67010200N-(4-{[tert-butyl(dimethyl)silyl]oxy}cyclohexyl)-1H-pyrazol-5-amine

生成物 1

HCID 178440648HCID 178440648、化合物収率 44%

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
HCID 7061N,N-Diethylaniline溶媒

反応条件

温度
70 °C

実験手順

A solution of N-(4-{[tert-butyl(dimethyl)silyl]oxy}cyclohexyl)-1H-pyrazol-5-amine (0.67 g), 1,8-diazabicyclo[5.4.0]undec-7-ene (0.067 mL) and methyl 2-{[6-(2-cyanophenyl)pyridin-3-yl]methyl}-3-oxoheptanoate (0.8 g) in diethylaniline (5 mL) was stirred at 180° C. for 5 hr. The mixture was allowed to cool, ethyl acetate and water were added, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated brine, dried over anhydrous magnesium sulfate, and concentrated. The residue was crudely purified by silica gel column chromatography. This was dissolved in tetrahydrofuran (4 mL). Tetrabutylammonium fluoride (2.5 mL) was added, and the mixture was stirred at 70° C. for 2 hr. The mixture was allowed to cool, ethyl acetate and saturated aqueous ammonium chloride solution were added, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated brine, dried over anhydrous magnesium sulfate, and concentrated. This was dissolved in acetonitrile (6 mL), 1,1,1-tris(acetyloxy)-1,1-dihydro-1,2-benziodoxol-3-(1H)-one (1.0 g) was added, and the mixture was stirred for 3 hr. Ethyl acetate, water and sodium thiosulfate were added to the reaction mixture, and the mixture was stirred for 30 min. After stirring, the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated. The residue was dissolved in ethanol (3 mL)-tetrahydrofuran (3 mL), and sodium borohydride (0.045 g) was added at 0° C. After stirring at 0° C. for 2 hr, ethyl acetate and then saturated aqueous ammonium chloride solution were added. The mixture was extracted with ethyl acetate, and the organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated. The residue was purified by silica gel column chromatography to give the title compound as a pale-yellow amorphous solid (0.48 g, 44%).

後処理

  1. temperatureto cool
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe organic layer was washed with water and saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated
  6. customThe residue was crudely purified by silica gel column chromatography
  7. dissolutionThis was dissolved in tetrahydrofuran (4 mL)
  8. additionTetrabutylammonium fluoride (2.5 mL) was added
  9. temperatureto cool
  10. additionethyl acetate and saturated aqueous ammonium chloride solution were added
  11. extractionthe mixture was extracted with ethyl acetate
  12. washThe organic layer was washed with water and saturated brine
  13. dry with materialdried over anhydrous magnesium sulfate
  14. concentrationconcentrated
  15. dissolutionThis was dissolved in acetonitrile (6 mL)
  16. addition1,1,1-tris(acetyloxy)-1,1-dihydro-1,2-benziodoxol-3-(1H)-one (1.0 g) was added
  17. stirringthe mixture was stirred for 3 hr
  18. additionEthyl acetate, water and sodium thiosulfate were added to the reaction mixture
  19. stirringthe mixture was stirred for 30 min
  20. stirringAfter stirring
  21. extractionthe mixture was extracted with ethyl acetate
  22. washThe organic layer was washed with saturated brine
  23. dry with materialdried over anhydrous magnesium sulfate
  24. customthe solvent was evaporated
  25. dissolutionThe residue was dissolved in ethanol (3 mL)-tetrahydrofuran (3 mL), and sodium borohydride (0.045 g)
  26. additionwas added at 0° C
  27. stirringAfter stirring at 0° C. for 2 hr
  28. additionethyl acetate and then saturated aqueous ammonium chloride solution were added
  29. extractionThe mixture was extracted with ethyl acetate
  30. washthe organic layer was washed with saturated brine
  31. dry with materialdried over anhydrous magnesium sulfate
  32. concentrationconcentrated
  33. customThe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-4bd7c393ba984c5a8bb62ed86557e0a0
出典データセット
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08592431B2

反応ノート

読み込み中…

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