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p-Toluenesulfonic acid → Azd3463

HRID 1256054
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HRID 1256054 반응식
Cl[C:2]1[N:7]=[C:6]([C:8]2[C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[NH:10][CH:9]=2)[C:5]([Cl:17])=[CH:4][N:3]=1.[NH2:18][C:19]1[CH:24]=[CH:23][C:22]([N:25]2[CH2:30][CH2:29][CH:28]([NH2:31])[CH2:27][CH2:26]2)=[CH:21][C:20]=1[O:32][CH3:33].CC1C=CC(S(O)(=O)=O)=CC=1>C(O)CCCC>[NH2:31][CH:28]1[CH2:29][CH2:30][N:25]([C:22]2[CH:23]=[CH:24][C:19]([NH:18][C:2]3[N:7]=[C:6]([C:8]4[C:16]5[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=5)[NH:10][CH:9]=4)[C:5]([Cl:17])=[CH:4][N:3]=3)=[C:20]([O:32][CH3:33])[CH:21]=2)[CH2:26][CH2:27]1
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참가 물질

5

반응물 3

HCID 6101p-Toluenesulfonic acidHCID 566553763-(2,5-Dichloropyrimidin-4-yl)-1H-indoleHCID 667101811-(4-Amino-3-methoxyphenyl)piperidin-4-amine

생성물 1

HCID 56599293Azd3463수율 36.2%

시약·촉매·용매 1

HCID 62761-Pentanol용매

반응 조건

온도
140 °C

실험 절차

A solution of 3-(2,5-dichloropyrimidin-4-yl)-1H-indole (5.28 g, 20 mmol), 1-(4-amino-3-methoxyphenyl)piperidin-4-amine (4.43 g, 20.00 mmol), and tosic acid (5.71 g, 30.00 mmol) in n-pentanol (40.0 ml) was placed in a round-bottomed flask. The solution was heated at 140° C., and stirred at that temperature for three days. The solvent was removed by concentration in vacuo, and to the residue was added sat. NaHCO3 solution and dichloromethane. The mixture was filtered and the obtained solid was dissolved in a mixture of THF and methanol and pre-absorbed on silica gel (120 g). The mixture was loaded onto silica gel column and eluted with 10% MeOH, 1% NH4OH in DCM. The collected fractions were concentrated, and the residue was triturated in diethyl ether. The collected solid after filtration was triturated in ethanol. Filtration afforded the title compound (3.25 g, 36.2% yield).

후처리

  1. customThe solvent was removed by concentration in vacuo
  2. additionto the residue was added sat. NaHCO3 solution and dichloromethane
  3. filtrationThe mixture was filtered
  4. dissolutionthe obtained solid was dissolved in a mixture of THF and methanol
  5. custompre-absorbed on silica gel (120 g)
  6. washeluted with 10% MeOH, 1% NH4OH in DCM
  7. concentrationThe collected fractions were concentrated
  8. customthe residue was triturated in diethyl ether
  9. filtrationThe collected solid after filtration
  10. customwas triturated in ethanol
  11. filtrationFiltration

출처 및 근거

ORD 기록
ord-d8ff5d3cf85947279f0dfec98f6fb564
출처 데이터셋
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08461170B2

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