Methyl iodide → 5,6,7,8-tetrahydro-5-oxo-1,7,7-trimethyl-2(1H)-quinolinone

HRID 1587001노트

반응식

HRID 1587001 반응식
[CH3:1][C:2]1([CH3:14])[CH2:11][C:10]2[NH:9][C:8](=[O:12])[CH:7]=[CH:6][C:5]=2[C:4](=[O:13])[CH2:3]1.CI.[C:17](=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[O:13]=[C:4]1[CH2:3][C:2]([CH3:14])([CH3:1])[CH2:11][C:10]2[N:9]([CH3:17])[C:8](=[O:12])[CH:7]=[CH:6][C:5]1=2

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 135163797,7-dimethyl-7,8-dihydroquinoline-2,5(1H,6H)-dione

생성물 1

HCID 190261755,6,7,8-tetrahydro-5-oxo-1,7,7-trimethyl-2(1H)-quinolinone수율 50.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 5,6,7,8-tetrahydro-7,7-dimethyl-5-oxo-2(1H)-quinolinone (15.0 g), methyl iodide (12.3 g), potassium carbonate (21.6 g), and dimethylformamide (230 ml) was stirred at room temperature for 21 hrs. The reaction mixture was filtered, and the filtrate was concentrated. Ethyl acetate was added to the residue, and the mixture was filtered. The filtrate was washed with brine, dried over anhydrous magnesium sulfate, filtered, and the filtrate was concentrated to give 8.1 g (50%) of 5,6,7,8-tetrahydro-5-oxo-1,7,7-trimethyl-2(1H)-quinolinone.

후처리

  1. filtrationThe reaction mixture was filtered
  2. concentrationthe filtrate was concentrated
  3. additionEthyl acetate was added to the residue
  4. filtrationthe mixture was filtered
  5. washThe filtrate was washed with brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. filtrationfiltered
  8. concentrationthe filtrate was concentrated

출처 및 근거

ORD 기록
ord-7c81b9949c8a4536b20e31229ed47a77
출처 데이터셋
uspto-grants-1993_06
특허 번호
US05216164

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