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Butyl bromide → 4-Butoxy-3-methoxybenzonitrile

HRID 1801477
ノート
印刷プレビュー

反応式

HRID 1801477 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([C:9]#[N:10])[CH:6]=[CH:5][C:4]=1[OH:11].C([O-])([O-])=O.[K+].[K+].[CH2:18](Br)[CH2:19][CH2:20][CH3:21]>CN(C=O)C>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([CH:6]=[CH:5][C:4]=1[O:11][CH2:18][CH2:19][CH2:20][CH3:21])[C:9]#[N:10]
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 8002Butyl bromideHCID 11430Potassium CarbonateHCID 781354-Hydroxy-3-methoxybenzonitrile

生成物 1

HCID 44587574-Butoxy-3-methoxybenzonitrile収率 105.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
37 °C

実験手順

2-methoxy-4-cyano-phenol (0.25 g, 1.67 mmol) and anhydrous DMF (2.00 mL) were added into a flask, then cooled in a water bath while stirring. Several batches of K2CO3 (0.347 g, 2.50 mmol) were added to the mixture and stirred at 20° C. to react for 1 h. n-butyl bromine (0.23 ml, 2.14 mmol) was added into the mixture, which was stirred at room temperature overnight, then heated at 37° C. to react for 6 h. Poured the solution into a mixture of ice/H2O (25 mL), then stirred for 10 min, a precipitate was formed. Filtered, washed with H2O, and air-dried to yield 0.361 g of white solid product with a recovery rate of 92%.

後処理

  1. temperaturecooled in a water bath
  2. stirringstirred at 20° C.
  3. additionwas added into the mixture, which
  4. stirringwas stirred at room temperature overnight
  5. customto react for 6 h
  6. additionPoured the solution
  7. stirringstirred for 10 min
  8. customa precipitate was formed
  9. filtrationFiltered
  10. washwashed with H2O
  11. customair-dried

出典と根拠

ORDレコード
ord-530c5479ce4140b091847314f7dece14
出典データセット
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08349835B2

反応ノート

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