Methyl iodide → HCID 21192515, 화합물

HRID 1067952노트

반응식

HRID 1067952 반응식
[C:1]([O:4][CH2:5][CH2:6][N:7]([CH2:24][CH3:25])[C:8]1[CH:9]=[C:10]2[C:15](=[CH:16][CH:17]=1)[N:14]=[CH:13][C:12]([C:18]([O:20][CH2:21][CH3:22])=[O:19])=[C:11]2[OH:23])(=[O:3])[CH3:2].[C:26](=O)([O-])[O-].[K+].[K+].IC>CN(C=O)C.ClCCl>[C:1]([O:4][CH2:5][CH2:6][N:7]([CH2:24][CH3:25])[C:8]1[CH:9]=[C:10]2[C:15](=[CH:16][CH:17]=1)[N:14]([CH3:26])[CH:13]=[C:12]([C:18]([O:20][CH2:21][CH3:22])=[O:19])[C:11]2=[O:23])(=[O:3])[CH3:2]

참가 물질

6

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 178469576HCID 178469576, 화합물

생성물 1

HCID 21192515HCID 21192515, 화합물수율 124.4%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 6344Dichloromethane용매

반응 조건

온도
90 °C

실험 절차

To a flask containing ethyl 6-[[2-(acetyloxy)ethyl](ethyl)amino]-4-hydroxy-3-quinolinecarboxylate (0.17 g) in DMF (5 mL) is added potassium carbonate (0.21 g) and iodomethane (0.05 mL). The reaction is tightly capped and heated to 90° C. After 3 hours, the reaction is cooled to room temperature, diluted with dichloromethane, filtered and concentrated under reduced pressure. The residue is adsorbed onto silica and chromatographed on silica eluting with 4% to 8% methanol in dichloromethane. The product-containing fractions are evaporated to give 0.22 g of the title compound as a orange solid.

후처리

  1. customThe reaction is tightly capped
  2. temperaturethe reaction is cooled to room temperature
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. customchromatographed on silica eluting with 4% to 8% methanol in dichloromethane
  6. customThe product-containing fractions are evaporated

출처 및 근거

ORD 기록
ord-2a106c0ded824393b30d1d8ebdfde5c6
출처 데이터셋
uspto-grants-2001_06
특허 번호
US06248739B1

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