Trifluoroacetic acid → HCID 22337014、化合物

HRID 585514ノート

反応式

HRID 585514 の反応式
C([SiH](CC)CC)C.C(O)(C(F)(F)F)=O.[NH2:15][C:16]1[CH:24]=[CH:23][CH:22]=[C:21]2[C:17]=1[CH:18](O)[N:19]([CH2:26][C:27]1[CH:28]=[C:29]([CH2:33][C:34]#[N:35])[CH:30]=[CH:31][CH:32]=1)[C:20]2=[O:25]>ClCCl>[NH2:15][C:16]1[CH:24]=[CH:23][CH:22]=[C:21]2[C:17]=1[CH2:18][N:19]([CH2:26][C:27]1[CH:28]=[C:29]([CH2:33][C:34]#[N:35])[CH:30]=[CH:31][CH:32]=1)[C:20]2=[O:25]

参加物

5

反応物 3

HCID 6422Trifluoroacetic acidHCID 12052TriethylsilaneHCID 22337029HCID 22337029、化合物

生成物 1

HCID 22337014HCID 22337014、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

At room temperature, initially 8 ml (50 mmol) of triethylsilane and then dropwise, 20 ml (260 mmol) of TFA are added to a suspension of 5.87 g (20 mmol, purity about 90%) of 2-{3-[(4-amino-3-hydroxy-1-oxo-1,3-dihydro-2H-isoindol-2-yl)methyl]phenyl}acetonitrile in 200 ml dichloromethane. The mixture is stirred at room temperature for 4 h and then concentrated and dried under high vacuum. The residue is taken up in dichloromethane and the mixture is washed with sat. sodium bicarbonate solution and sat. sodium chloride solution, dried over magnesium sulfate and concentrated to about 50 ml. About 100 ml of ether are added to the crystal slurry, which is then stirred for about 2 h and filtered. Yield: 4.36 g (78.7% of theory);

後処理

  1. concentrationconcentrated
  2. customdried under high vacuum
  3. washthe mixture is washed with sat. sodium bicarbonate solution and sat. sodium chloride solution
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated to about 50 ml
  6. additionAbout 100 ml of ether are added to the crystal slurry, which
  7. stirringis then stirred for about 2 h
  8. filtrationfiltered

出典と根拠

ORDレコード
ord-24f03be43eff4cf487f4b3fcbe7c91ac
出典データセット
uspto-grants-2005_08
特許番号
US06933295B2

反応ノート

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