Trifluoroacetic acid → HCID 22337014, 화합물

HRID 585514노트

반응식

HRID 585514 반응식
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]

참가 물질

5

반응물 3

HCID 6422Trifluoroacetic acidHCID 12052TriethylsilaneHCID 22337029HCID 22337029, 화합물

생성물 1

HCID 22337014HCID 22337014, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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);

후처리

  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

출처 및 근거

ORD 기록
ord-24f03be43eff4cf487f4b3fcbe7c91ac
출처 데이터셋
uspto-grants-2005_08
특허 번호
US06933295B2

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