Trifluoroacetic acid → 5-(6-(4-aminopiperidin-1-yl)pyridin-3-yl)-3-(ethyl(tetrahydro-2H-pyran-4-yl)amino)-N-((4-isopropyl-6-methyl-2-oxo-1,2-dihydropyridin-3-yl)methyl)-2-methylbenzamide

HRID 1616514ノート

反応式

HRID 1616514 の反応式
[CH2:1]([N:3]([CH:46]1[CH2:51][CH2:50][O:49][CH2:48][CH2:47]1)[C:4]1[CH:5]=[C:6]([C:26]2[CH:27]=[CH:28][C:29]([N:32]3[CH2:37][CH2:36][CH:35]([NH:38]C(=O)OC(C)(C)C)[CH2:34][CH2:33]3)=[N:30][CH:31]=2)[CH:7]=[C:8]([C:11](=[O:25])[NH:12][CH2:13][C:14]2[C:15](=[O:24])[NH:16][C:17]([CH3:23])=[CH:18][C:19]=2[CH:20]([CH3:22])[CH3:21])[C:9]=1[CH3:10])[CH3:2].C(O)(C(F)(F)F)=O>C(Cl)Cl>[NH2:38][CH:35]1[CH2:34][CH2:33][N:32]([C:29]2[N:30]=[CH:31][C:26]([C:6]3[CH:5]=[C:4]([N:3]([CH2:1][CH3:2])[CH:46]4[CH2:47][CH2:48][O:49][CH2:50][CH2:51]4)[C:9]([CH3:10])=[C:8]([CH:7]=3)[C:11]([NH:12][CH2:13][C:14]3[C:15](=[O:24])[NH:16][C:17]([CH3:23])=[CH:18][C:19]=3[CH:20]([CH3:22])[CH3:21])=[O:25])=[CH:27][CH:28]=2)[CH2:37][CH2:36]1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 86672674tert-butyl (1-(5-(3-(ethyl(tetrahydro-2H-pyran-4-yl)amino)-5-(((4-isopropyl-6-methyl-2-oxo-1,2-dihydropyridin-3-yl)methyl)carbamoyl)-4-methylphenyl)pyridin-2-yl)piperidin-4-yl)carbamate

生成物 1

HCID 708727265-(6-(4-aminopiperidin-1-yl)pyridin-3-yl)-3-(ethyl(tetrahydro-2H-pyran-4-yl)amino)-N-((4-isopropyl-6-methyl-2-oxo-1,2-dihydropyridin-3-yl)methyl)-2-methylbenzamide収率 98.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

tert-butyl (1-(5-(3-(ethyl(tetrahydro-2H-pyran-4-yl)amino)-5-(((4-isopropyl-6-methyl-2-oxo-1,2-dihydropyridin-3-yl)methyl)carbamoyl)-4-methylphenyl)pyridin-2-yl)piperidin-4-yl)carbamate (0.31 g, 0.44 mmol) was taken in DCM (5 mL) and TFA (1 mL) was added to it and stirred at rt for 2 h. After completion of reaction, solvent was removed under reduced pressure and saturated NaHCO3 solution was added to it. Extraction was carried out using 10% MeOH/DCM; the combined organic layers were washed with water and brine; dried over anhydrous Na2SO4; filtered and concentrated under reduced pressure to give the title compound (0.26 g, 98.11%)

後処理

  1. customAfter completion of reaction, solvent
  2. customwas removed under reduced pressure and saturated NaHCO3 solution
  3. additionwas added to it
  4. extractionExtraction
  5. washthe combined organic layers were washed with water and brine
  6. dry with materialdried over anhydrous Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-dad4043da1ff43938f1b257aaf2da62e
出典データセット
uspto-grants-2014_07
特許番号
US08765732B2

反応ノート

読み込み中…