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o-Chlorophenylacetic acid → Acetyl chloride, 2-(2-chlorophenyl)-

HRID 54748
ノート
印刷プレビュー

反応式

HRID 54748 の反応式
S(Cl)([Cl:3])=O.[Cl:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[CH2:12][C:13]([OH:15])=O>>[Cl:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[CH2:12][C:13]([Cl:3])=[O:15]
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

HCID 17124o-Chlorophenylacetic acidHCID 24386Thionyl Chloride

生成物 1

HCID 182669Acetyl chloride, 2-(2-chlorophenyl)-

実験手順

15 ml of thionyl chloride was added to 0.44 g of 2-chlorophenylacetic acid. The mixture was stirred at room temperature for 2 hours. The reaction mixture was subjected to distillation to remove the remaining thionyl chloride and then to azeotropy with toluene twice to completely remove the thionyl chloride. The residue was dissolved in 10 ml of dichloromethane. 0.36 ml of triethylamine was added, with ice-cooling, to a dichloromethane solution containing 0.40 g of 5-dimethylamino-1-(4-aminobenzoyl)-2,3,4,5-tetrahydro-1H-benzoazepine. Thereto was dropwise added the above obtained 2-(2-chlorophenyl)acetyl chloride solution. The resulting mixture was stirred at room temperature for 1 hour. The reaction mixture was water-washed twice, then dried over magnesium sulfate and concentrated. The residue was purified by silica gel column chromatography (elutant: chloroform/methanol=200/1) and then recrystallized from methanol-diethyl ether to obtain 0.29 g of 5-dimethylamino-1-{4-[2-(2-chlorophenyl)acetylamino]benzoyl}-2,3,4,5-tetrahydro-1H-benzoazepine.

後処理

  1. distillationThe reaction mixture was subjected to distillation
  2. customto remove the remaining thionyl chloride
  3. customto completely remove the thionyl chloride
  4. dissolutionThe residue was dissolved in 10 ml of dichloromethane
  5. addition0.36 ml of triethylamine was added, with ice-
  6. temperaturecooling, to a dichloromethane solution
  7. additioncontaining 0.40 g of 5-dimethylamino-1-(4-aminobenzoyl)-2,3,4,5-tetrahydro-1H-benzoazepine
  8. additionThereto was dropwise added the

出典と根拠

ORDレコード
ord-d0c460ed1540444c85bf2a050d61eee3
出典データセット
uspto-grants-1997_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05622947

反応ノート

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