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Dimethylformamide → N-Pyridin-2-yl-N~2~-[1-(trifluoroacetyl)piperidin-4-yl]glycinamide

HRID 2193048
ノート
印刷プレビュー

反応式

HRID 2193048 の反応式
CN(C)C=O.Cl.[F:7][C:8]([F:19])([F:18])[C:9]([N:11]1[CH2:16][CH2:15][CH:14]([NH2:17])[CH2:13][CH2:12]1)=[O:10].Br[CH2:21][C:22]([NH:24][C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][N:26]=1)=[O:23].C(=O)([O-])[O-].[K+].[K+]>O.C(OCC)(=O)C>[N:26]1[CH:27]=[CH:28][CH:29]=[CH:30][C:25]=1[NH:24][C:22](=[O:23])[CH2:21][NH:17][CH:14]1[CH2:15][CH2:16][N:11]([C:9](=[O:10])[C:8]([F:7])([F:18])[F:19])[CH2:12][CH2:13]1
参加物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 6228DimethylformamideHCID 11430Potassium CarbonateHCID 34158372-bromo-N-pyridin-2-yl-acetamideHCID 866331901-(4-Aminopiperidin-1-YL)-2,2,2-trifluoroethan-1-one hydrochloride

生成物 1

HCID 59398027N-Pyridin-2-yl-N~2~-[1-(trifluoroacetyl)piperidin-4-yl]glycinamide

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

To 15 mL of an N,N-dimethylformamide solution containing 1.5 g of 1-(trifluoroacetyl)piperidine-4-amine hydrochloride, 1.4 g of 2-bromo-N-(pyridin-2-yl)acetamide and 1.8 g of potassium carbonate were added, and the mixture was stirred at room temperature for 4 hours. The reaction mixture was added with ethyl acetate and water. The organic layer was separated, and the aqueous layer was extracted with ethyl acetate. The organic layer and the extract were combined, the resultant solution was washed sequentially with water and an aqueous saturated sodium chloride solution and dried over anhydrous magnesium sulfate, and the solvent was removed under reduced pressure. The residue thus obtained was purified by silica gel column chromatography [eluent; chloroform:methanol=10:1] to obtain 1.1 g of a light brown oily substance, N-(pyridin-2-yl)-N2-(1-(trifluoroacetyl)piperidin-4-yl)glycinamide.

後処理

  1. additionwere added
  2. customThe organic layer was separated
  3. extractionthe aqueous layer was extracted with ethyl acetate
  4. washthe resultant solution was washed sequentially with water
  5. dry with materialan aqueous saturated sodium chloride solution and dried over anhydrous magnesium sulfate
  6. customthe solvent was removed under reduced pressure
  7. customThe residue thus obtained
  8. customwas purified by silica gel column chromatography [eluent; chloroform:methanol=10:1]

出典と根拠

ORDレコード
ord-6f94c368614d4dfca23aa6b35ab55a2f
出典データセット
uspto-grants-2012_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08329694B2

反応ノート

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