Acetic Anhydride → 2,3-Dihydro-5-hydroxy-4,7-dimethyl-1H-indole-1-carbaldehyde

HRID 985578노트

반응식

HRID 985578 반응식
[C:1](OC(=O)C)(=[O:3])C.[CH3:8][C:9]1[C:17]([OH:18])=[CH:16][C:15]([CH3:19])=[C:14]2[C:10]=1[CH2:11][CH2:12][NH:13]2>C(O)=O>[OH:18][C:17]1[C:9]([CH3:8])=[C:10]2[C:14](=[C:15]([CH3:19])[CH:16]=1)[N:13]([CH:1]=[O:3])[CH2:12][CH2:11]2

참가 물질

4

반응물 2

HCID 7918Acetic AnhydrideHCID 225068232,3-Dihydro-4,7-dimethyl-1H-indol-5-ol

생성물 1

HCID 225068342,3-Dihydro-5-hydroxy-4,7-dimethyl-1H-indole-1-carbaldehyde수율 37%

시약·촉매·용매 1

HCID 284Formic Acid용매

실험 절차

Acetic anhydride (25 ml, 264 mmol) was added at room temperature to formic acid (75 ml) and stirred for 30 minutes. To the solution, 2,3-dihydro-4,7-dimethyl-1H-indol-5-ol (14.4 g, 88 mmol) was added and the mixture was stirred for 2 hours. The reaction mixture was concentrated under reduced pressure, and the residue was dissolved in a chloroform methanol solution and washed: with a saturated aqueous solution of sodium hydrogen carbonate. The organic layer was washed with saturated brine and dried over sodium sulfate, and then the solvent was removed under reduced pressure. The resultant residue was washed with diisopropyl ether to obtain 6.2 g of the title compound.

후처리

  1. stirringthe mixture was stirred for 2 hours
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. dissolutionthe residue was dissolved in a chloroform methanol solution
  4. washwashed
  5. washThe organic layer was washed with saturated brine
  6. dry with materialdried over sodium sulfate
  7. customthe solvent was removed under reduced pressure
  8. washThe resultant residue was washed with diisopropyl ether

출처 및 근거

ORD 기록
ord-2a85e356c7dd40b5b12ef041fd5f8ebc
출처 데이터셋
uspto-grants-2005_03
특허 번호
US06872718B1

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