p-Toluenesulfonic acid → HCID 178428862、化合物

HRID 488726ノート

反応式

HRID 488726 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][N:5]=[CH:4][C:3]=1[C:8]1[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][C:9]=1[Cl:15].C([O:19][CH2:20][CH3:21])(=O)C.[C:22]1(C)C=CC(S(O)(=O)=O)=C[CH:23]=1>C1C=CC=CC=1>[CH3:22][C:23]1[CH:21]=[C:20]([OH:19])[C:7]2[C:2](=[C:3]([C:8]3[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][C:9]=3[Cl:15])[CH:4]=[N:5][CH:6]=2)[N:1]=1

参加物

5

反応物 3

HCID 6101p-Toluenesulfonic acidHCID 8857Ethyl AcetateHCID 222673263-(2,4-Dichlorophenyl)pyridin-4-amine

生成物 1

HCID 178428862HCID 178428862、化合物

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

A solution of B1 (2.41 g, 10.1 mmole), ethyl acetate (1.31 g, 10.1 mmole) and p-toluenesulfonic acid (70 mg) in benzene (50 ml) is heated at reflux for 2 h. during which 10 ml of solvent is removed by distillation. After evaporation, the residue is added to boiling diphenyl ether (10 ml) and heating is continued for 1 h; then the solution is cooled and poured into high boiling petroleum ether with vigorous stirring. The resulting solid formed is filtered off and washed with diethyl ether to give the product B2.

後処理

  1. customis removed by distillation
  2. customAfter evaporation
  3. additionthe residue is added
  4. temperatureheating
  5. temperaturethen the solution is cooled
  6. additionpoured
  7. customThe resulting solid formed
  8. filtrationis filtered off
  9. washwashed with diethyl ether

出典と根拠

ORDレコード
ord-f82d02bce378407597b41adcb05d8c71
出典データセット
uspto-grants-2005_12
特許番号
US06974808B2

反応ノート

読み込み中…