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Chlorobenzene → 3,8-Dimethyl-5-hydroxycarbostyril

HRID 1900807
ノート
印刷プレビュー

反応式

HRID 1900807 の反応式
C[O:2][C:3]1[CH:4]=[CH:5][C:6]([CH3:21])=[C:7]([NH:9][C:10](=[O:20])[C:11]([CH3:19])=[CH:12]C2C=CC=CC=2)[CH:8]=1.[Cl-].[Al+3].[Cl-].[Cl-].ClC1C=CC=CC=1>CCCCCC>[OH:2][C:3]1[CH:4]=[CH:5][C:6]([CH3:21])=[C:7]2[C:8]=1[CH:19]=[C:11]([CH3:12])[C:10](=[O:20])[NH:9]2
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 7964ChlorobenzeneHCID 6451240Aluminum(III) ChlorideHCID 54285619N-(5-Methoxy-2-methylphenyl)alpha-methylcinnamamide

生成物 1

HCID 233696243,8-Dimethyl-5-hydroxycarbostyril収率 85.3%

試薬・触媒・溶媒 1

HCID 8058Hexane溶媒

反応条件

温度
125 °C

実験手順

N-(5-Methoxy-2-methylphenyl)α-methylcinnamamide (21.3 g, 75.8 mmol) and aluminum chloride (50.4 g, 378 mmol) were combined with chlorobenzene (158 ml), and heated in a bath at 125° C. for 45 minutes while stirring. After cooling, the mixture was poured into ice-water, to which hexane was added. Precipitated crystals were collected by filtration, and dissolved in chloroform-methanol (4:1). After drying and condensing, the resultant residue was washed with chloroform to obtain 12.22 g of the title compound as pale brown crystals (85.3%).

後処理

  1. temperatureAfter cooling
  2. additionwas added
  3. customPrecipitated crystals
  4. filtrationwere collected by filtration
  5. dissolutiondissolved in chloroform-methanol (4:1)
  6. customAfter drying
  7. customcondensing
  8. washthe resultant residue was washed with chloroform

出典と根拠

ORDレコード
ord-985f4521d72045a2998b995cc89f35cb
出典データセット
uspto-grants-1996_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05576324

反応ノート

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