p-Toluenesulfonic acid → HCID 178428862, 화합물

HRID 488726노트

반응식

HRID 488726 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 178428862HCID 178428862, 화합물

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f82d02bce378407597b41adcb05d8c71
출처 데이터셋
uspto-grants-2005_12
특허 번호
US06974808B2

반응 노트

불러오는 중…