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Oxalyl chloride → Methyl 2,6-dichloro-5-fluoronicotinate

HRID 368465
ノート
印刷プレビュー

反応式

HRID 368465 の反応式
[Cl:1][C:2]1[N:10]=[C:9]([Cl:11])[C:8]([F:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[C:13](Cl)(=O)C(Cl)=O>CN(C)C=O.ClCCl>[Cl:1][C:2]1[N:10]=[C:9]([Cl:11])[C:8]([F:12])=[CH:7][C:3]=1[C:4]([O:6][CH3:13])=[O:5]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 65578Oxalyl chlorideHCID 27336592,6-Dichloro-5-fluoronicotinic acid

生成物 1

HCID 2775354Methyl 2,6-dichloro-5-fluoronicotinate

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide触媒HCID 6344Dichloromethane溶媒

実験手順

To 60 ml of dichloromethane were added 21.0 g of 2,6-dichloro-5-fluoronicotinic acid, 10 ml of oxalylchloride, and 10 drops of N,N-dimethylformamide, and the mixture was stirred at room temperature for one day. The solvent and the excess reagents were distilled off under reduced pressure, and the residue was dissolved in 50 ml of chloroform. 10 ml of methanol was added dropwise to the solution, and the solution was stirred at room temperature for 60 minutes, and 15 g of anhydrous potassium carbonate was added to the solution and the solution was stirred for another 30 minutes. The solution was separated by adding 150 ml of chloroform and 150 ml of distilled water, and the chloroform layer was dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to obtain 26.6 g of the title compound as a colorless crude oily residue.

後処理

  1. distillationThe solvent and the excess reagents were distilled off under reduced pressure
  2. dissolutionthe residue was dissolved in 50 ml of chloroform
  3. addition10 ml of methanol was added dropwise to the solution
  4. stirringthe solution was stirred at room temperature for 60 minutes
  5. addition15 g of anhydrous potassium carbonate was added to the solution
  6. stirringthe solution was stirred for another 30 minutes
  7. customThe solution was separated
  8. additionby adding 150 ml of chloroform and 150 ml of distilled water
  9. dry with materialthe chloroform layer was dried over anhydrous magnesium sulfate
  10. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-eb7a876783504d67882984210c380e6e
出典データセット
uspto-grants-2000_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06133284

反応ノート

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