Ethyl Acetate → 2,4-Dimethoxy-5-fluoronitrobenzene

HRID 649854

反応式

HRID 649854 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[CH:6]=[CH:5][C:4]=1[N+:11]([O-:13])=[O:12].[O-]S(C(F)(F)[F:19])(=O)=O.ClC1C=[N+](F)C=C(Cl)C=1.C(OCC)(=O)C>ClCC(Cl)(Cl)Cl>[F:19][C:6]1[CH:5]=[C:4]([N+:11]([O-:13])=[O:12])[C:3]([O:2][CH3:1])=[CH:8][C:7]=1[O:9][CH3:10]

参加物

5

反応物 3

HCID 8857Ethyl AcetateHCID 786332,4-Dimethoxy-1-nitrobenzeneHCID 27245783,5-Dichloro-1-fluoropyridinium triflate2 回

生成物 1

HCID 27584142,4-Dimethoxy-5-fluoronitrobenzene

試薬・触媒・溶媒 1

HCID 124181,1,1,2-Tetrachloroethane溶媒

反応条件

温度
120 °C

実験手順

To a solution of 2,4-dimethoxy-nitrobenzene (1.0 g) in tetrachloroethane (10 mL) is added 3,5-dichloro-1-fluoro-pyridinium triflate (85%, 5.07 g) and the mixture is heated to 120° C. for 5 hours. Additional 3,5-dichloro-1-fluoro-pyridinium triflate (85%, 0.25 g) is added and heating is continued for 1 hour. The solution is then cooled to room temperature and passed over a column of silica gel (hexanes followed by 30% ethyl acetate in hexanes is used as the eluant). Product containing fractions are combined, evaporated under reduced pressure, and the residue is crystallized from hexanes to provide the desired product as a tan solid.

後処理

  1. temperatureheating
  2. temperatureThe solution is then cooled to room temperature
  3. additionProduct containing fractions
  4. customevaporated under reduced pressure
  5. customthe residue is crystallized from hexanes

出典と根拠

ORDレコード
ord-beefefe3761740c4b3b00c80aa88b061
出典データセット
uspto-grants-2001_08
特許番号
US06271236B1

関連ノート

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