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

HRID 618541

反応式

HRID 618541 の反応式
[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

参加物

6

反応物 3

HCID 143137-MethylisatinHCID 102312Benzyloxyamine hydrochlorideHCID 517045Sodium Acetate

生成物 1

HCID 1361447423-(Benzyloxyimino)-7-methylindolin-2-one収率 68%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ca88e2b2befa45cbbfd7e0a2a3a2a6bd
出典データセット
uspto-grants-1999_09
特許番号
US05952511

関連ノート

読み込み中…