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Potassium Carbonate → 1-Ethynyl-2-methoxybenzene

HRID 1814479
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HRID 1814479 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[C:9]#[C:10]C1C=CC(OC)=CC=1C=O.Cl.NO.C([O-])(=O)C.[Na+].C(=O)([O-])[O-].[K+].[K+]>C(O)C.O>[C:9]([C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=1[O:2][CH3:1])#[CH:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 11430Potassium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 225030652-[2-(2-Methoxyphenyl)-ethynyl]-5-methoxybenzaldehyde

생성물 1

HCID 5829121-Ethynyl-2-methoxybenzene수율 127.3%

시약·촉매·용매 2

HCID 702Ethanol
용매
HCID 962Water용매

실험 절차

2-[2-(2-Methoxyphenyl)-ethynyl]-5-methoxybenzaldehyde (0.95 g), hydroxylamine hydrochloride (0.25 g) and sodium acetate (0.32 g) were reacted in ethanol (20 ml) at 60° C. for 2 hr. Potassium carbonate (0.6 g) and water (2 ml) were added to the reaction mixture, and the mixture was heated under reflux for 12 hr. The reaction solution was evaporated, and then the resulting residue was extracted with methylene chloride, washed with brine and dried. The solvent was removed, and the resulting residue was purified by silica gel column chromatography (methylene chloride/methanol system), to give 0.60 g of the title compound as a yellowish brown amorphous. (232-4) 1-Chloro-7-methoxy-3-(2-methoxyphenyl)isoquinoline

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 12 hr
  3. customThe reaction solution was evaporated
  4. extractionthe resulting residue was extracted with methylene chloride
  5. washwashed with brine
  6. customdried
  7. customThe solvent was removed
  8. customthe resulting residue was purified by silica gel column chromatography (methylene chloride/methanol system)

출처 및 근거

ORD 기록
ord-ad56733f83d14c14800aef62f052aa63
출처 데이터셋
uspto-grants-2005_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06875761B2

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