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Methane, dichloromethoxy- → 8-Methoxy-1-methyl-2-oxo-1,2,3,4-tetrahydroquinoline-5-carboxaldehyde

HRID 503986
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HRID 503986 반응식
[CH3:1][O:2][C:3]1[CH:4]=[CH:5][CH:6]=[C:7]2[C:12]=1[N:11]([CH3:13])[C:10](=[O:14])[CH2:9][CH2:8]2.[CH3:15][O:16]C(Cl)Cl>ClCCl.[Ti](Cl)(Cl)(Cl)Cl>[CH3:1][O:2][C:3]1[C:12]2[N:11]([CH3:13])[C:10](=[O:14])[CH2:9][CH2:8][C:7]=2[C:6]([CH:15]=[O:16])=[CH:5][CH:4]=1
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참가 물질

5

반응물 2

HCID 21004Methane, dichloromethoxy-2회HCID 133841968-methoxy-1-methyl-3,4-dihydro-1H-quinolin-2-one

생성물 1

HCID 866139148-Methoxy-1-methyl-2-oxo-1,2,3,4-tetrahydroquinoline-5-carboxaldehyde수율 80%

시약·촉매·용매 2

HCID 24193Titanium Tetrachloride촉매2회HCID 6344Dichloromethane용매

실험 절차

8-Methoxy-1-methyl-3,4-dihydro-1H-quinolin-2-one (1.5 g) was dissolved in dichloromethane (15 ml), and dichloromethyl methyl ether (0.86 ml) was added at room temperature, followed by cooling with ice water. Titanium tetrachloride (10.5 ml) was added dropwise, and the resulting mixture was stirred at room temperature overnight. Further, dichloromethyl methyl ether (1.29 ml) and titanium tetrachloride (15.8 ml) were added, and stirring was carried out at room temperature for 5 hours. The reaction mixture was poured into ice water, and the aqueous layer was subjected to extraction with dichloromethane. The organic layer was dried over sodium sulfate, filtered, and concentrated under reduced pressure. Hexane was added to the residue, and the produced insoluble matter was collected by filtration and dried to thereby obtain 1.37 g (yield: 80%) of 8-methoxy-1-methyl-2-oxo-1,2,3,4-tetrahydroquinoline-5-carboxaldehyde.

후처리

  1. stirringstirring
  2. waitwas carried out at room temperature for 5 hours
  3. extractionthe aqueous layer was subjected to extraction with dichloromethane
  4. dry with materialThe organic layer was dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. additionHexane was added to the residue
  8. filtrationthe produced insoluble matter was collected by filtration
  9. customdried

출처 및 근거

ORD 기록
ord-89e8987d647d402aa7840a1b1285fb16
출처 데이터셋
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07777038B2

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