Dichloromethane → 4-(Benzyloxy)-2-fluorobenzonitrile

HRID 1456360ノート

反応式

HRID 1456360 の反応式
[CH2:1](Br)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[F:15][C:16]1[CH:23]=[C:22]([OH:24])[CH:21]=[CH:20][C:17]=1[C:18]#[N:19].ClCCl>C(#N)C>[F:15][C:16]1[CH:23]=[C:22]([O:24][CH2:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[CH:21]=[CH:20][C:17]=1[C:18]#[N:19]

参加物

6

反応物 4

HCID 6344DichloromethaneHCID 7498Benzyl BromideHCID 11430Potassium CarbonateHCID 27346752-Fluoro-4-hydroxybenzonitrile

生成物 1

HCID 113336284-(Benzyloxy)-2-fluorobenzonitrile収率 84.3%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

15.2 ml (0.127 mol) of benzyl bromide and 29.3 g (0.212 mol) of potassium carbonate are added to a solution of 13.3 g (0.106 mol) of 2-fluoro-4-hydroxybenzonitrile in 150 ml of acetonitrile. The mixture is stirred at reflux for 1 hour 30 minutes and then filtered, the filtrate is concentrated under reduced pressure, and the oil obtained is diluted in the minimum amount of dichloromethane. After crystallization by addition of diisopropyl ether, filtration and drying, 20.3 g of product are obtained. Melting point : 87° C.

後処理

  1. temperatureat reflux for 1 hour 30 minutes
  2. filtrationfiltered
  3. concentrationthe filtrate is concentrated under reduced pressure
  4. customthe oil obtained
  5. customAfter crystallization
  6. additionby addition of diisopropyl ether, filtration
  7. customdrying

出典と根拠

ORDレコード
ord-896ec0e06715400fa274248c5d1f7a22
出典データセット
uspto-grants-1998_12
特許番号
US05843975

反応ノート

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