7-Methylisatin → 3-(Benzyloxyimino)-7-methylindolin-2-one

HRID 618541

반응식

HRID 618541 반응식
[CH3:1][C:2]1[CH:3]=[CH:4][CH:5]=[C:6]2[C:10]=1[NH:9][C:8](=[O:11])[C:7]2=O.Cl.[CH2:14]([O:21][NH2:22])[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.C([O-])(=O)C.[Na+]>C(O)C.O>[CH2:14]([O:21][N:22]=[C:7]1[C:6]2[C:10](=[C:2]([CH3:1])[CH:3]=[CH:4][CH:5]=2)[NH:9][C:8]1=[O:11])[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1

참가 물질

6

반응물 3

HCID 143137-MethylisatinHCID 102312Benzyloxyamine hydrochlorideHCID 517045Sodium Acetate

생성물 1

HCID 1361447423-(Benzyloxyimino)-7-methylindolin-2-one수율 68%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

To a suspension of 4.91 g of 7-methylisatin in 100 ml of ethanol was added a solution of 5.59 g of O-benzylhydroxylamine hydrochloride and 3.29 g of sodium acetate in 40 ml of water at room temperature. The mixture was stirred at room temperature for 3 hours and concentrated. The concentrate was diluted with chloroform and washed with water. The organic layer was dried over anhydrous sodium sulfate and concentrated. Recrystallization of the crude product from benzene yielded 5.40 g (68%) of the title compound.

후처리

  1. concentrationconcentrated
  2. additionThe concentrate was diluted with chloroform
  3. washwashed with water
  4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  5. concentrationconcentrated
  6. customRecrystallization of the crude product from benzene

출처 및 근거

ORD 기록
ord-ca88e2b2befa45cbbfd7e0a2a3a2a6bd
출처 데이터셋
uspto-grants-1999_09
특허 번호
US05952511

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