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Water → 3,8-Dimethyl-5-(2-butenyloxy)carbostyril

HRID 1900827
ノート
印刷プレビュー

反応式

HRID 1900827 の反応式
[CH3:1][C:2]1[C:3](=[O:14])[NH:4][C:5]2[C:10]([CH:11]=1)=[C:9]([OH:12])[CH:8]=[CH:7][C:6]=2[CH3:13].[CH2:15](Br)[CH:16]=[CH:17][CH3:18].C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[CH3:1][C:2]1[C:3](=[O:14])[NH:4][C:5]2[C:10]([CH:11]=1)=[C:9]([O:12][CH2:15][CH:16]=[CH:17][CH3:18])[CH:8]=[CH:7][C:6]=2[CH3:13]
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

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 1224142-Butene, 1-bromo-HCID 233696243,8-Dimethyl-5-hydroxycarbostyril

生成物 1

HCID 545443253,8-Dimethyl-5-(2-butenyloxy)carbostyril収率 63%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
70 °C

実験手順

3,8-Dimethyl-5-hydroxycarbostyril (3 g, 15.86 mmol) was dissolved in dimethylformamide (30 ml). To the solution, crotyl bromide (2.06 ml, 20.45 mmol) and potassium carbonate (4.4g, 31.84 mmol) were added. The mixture was stirred at 70° C. for 2 hours. After spontaneous cooling, water (90 ml) was added to the mixture. Precipitated crystals were collected by filtration. The obtained crystals were dissolved in chloroform, washed with water and saturated aqueous NaCl solution in this order, and dried. The solvent was distilled off under reduced pressure, and the residue was recrystallized from chloroform-n-hexane. As a result, 2.43 g of the title compound was obtained as colorless crystals (63%).

後処理

  1. customPrecipitated crystals
  2. filtrationwere collected by filtration
  3. dissolutionThe obtained crystals were dissolved in chloroform
  4. washwashed with water and saturated aqueous NaCl solution in this order
  5. customdried
  6. distillationThe solvent was distilled off under reduced pressure
  7. customthe residue was recrystallized from chloroform-n-hexane

出典と根拠

ORDレコード
ord-53f1a79e0f474c6291c5c4afa2991c7f
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

読み込み中…

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