Acetic Anhydride → 1H-Indole-2,3-dione, 1-acetyl-5-methyl-

HRID 6359

반응식

HRID 6359 반응식
[CH3:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[NH:7][C:6](=[O:11])[C:5]2=[O:12].[H-].[Na+].[C:15](OC(=O)C)(=[O:17])[CH3:16].C(=O)(O)[O-].[Na+]>C1(C)C=CC=CC=1>[C:15]([N:7]1[C:8]2[C:4](=[CH:3][C:2]([CH3:1])=[CH:10][CH:9]=2)[C:5](=[O:12])[C:6]1=[O:11])(=[O:17])[CH3:16]

참가 물질

6

반응물 4

HCID 7918Acetic AnhydrideHCID 118405-MethylisatinHCID 24758Sodium hydrideHCID 516892Sodium Bicarbonate

생성물 1

HCID 5399471H-Indole-2,3-dione, 1-acetyl-5-methyl-수율 47.6%

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
0 °C

실험 절차

With stirring at 0° C., 8.06 g (50.0 mmols) of 5-methylisatin was added by small portions to a solution of 2.00 g (50.0 mmols) of sodium hydride in toluene. While stirring under ice cooling, 4.7 ml (50.0 mmols) of acetic anhydride was dropwise added to the mixture followed by heating at 80° C. for further an hour with stirring. After completion of the reaction, an aqueous saturated sodium bicarbonate solution was added to the reaction mixture. The crystals were filtered, washed with water and dried to give 4.84 g (yield, 47%) of 1-acetyl-5-methylisatin.

후처리

  1. stirringWhile stirring under ice cooling
  2. temperatureby heating at 80° C. for further an hour
  3. stirringwith stirring
  4. customAfter completion of the reaction
  5. filtrationThe crystals were filtered
  6. washwashed with water
  7. customdried

출처 및 근거

ORD 기록
ord-b0cbbbccef144c919960c98519e95613
출처 데이터셋
uspto-grants-1993_09
특허 번호
US05248684

연결된 노트

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