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Potassium Carbonate → 1-Ethynyl-2-methoxybenzene

HRID 1814479
ノート
印刷プレビュー

反応式

HRID 1814479 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

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

生成物 1

HCID 5829121-Ethynyl-2-methoxybenzene収率 127.3%

試薬・触媒・溶媒 2

HCID 702Ethanol
溶媒
HCID 962Water溶媒

実験手順

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

後処理

  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)

出典と根拠

ORDレコード
ord-ad56733f83d14c14800aef62f052aa63
出典データセット
uspto-grants-2005_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06875761B2

反応ノート

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