3-Fluorobenzylamine → N-(3-fluorobenzyl)-2-[(pyridin-3-ylamino)sulfonyl]benzamide

HRID 252216

반응식

HRID 252216 반응식
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([NH:7][S:8]([C:11]2[CH:20]=[CH:19][CH:18]=[CH:17][C:12]=2[C:13]([O:15]C)=O)(=[O:10])=[O:9])[CH:2]=1.[F:21][C:22]1[CH:23]=[C:24]([CH:27]=[CH:28][CH:29]=1)[CH2:25][NH2:26]>>[F:21][C:22]1[CH:23]=[C:24]([CH:27]=[CH:28][CH:29]=1)[CH2:25][NH:26][C:13](=[O:15])[C:12]1[CH:17]=[CH:18][CH:19]=[CH:20][C:11]=1[S:8]([NH:7][C:3]1[CH:2]=[N:1][CH:6]=[CH:5][CH:4]=1)(=[O:9])=[O:10]

참가 물질

3

반응물 2

HCID 668533-FluorobenzylamineHCID 4354882Methyl 2-[(pyridin-3-ylamino)sulfonyl]benzoate

생성물 1

HCID 58924173N-(3-fluorobenzyl)-2-[(pyridin-3-ylamino)sulfonyl]benzamide수율 84%

실험 절차

The title compound was prepared according to procedures described above, using methyl 2-[(pyridin-3-ylamino)sulfonyl]benzoate and 3-fluorobenzylamine. The title compound was further purified by dissolving 25 g in EtOH (300 mL) and gently heating using water bath to 80° C. The resulting solids material were then slowly dissolved and more EtOH (50 mL) was added to completely dissolve all the solids. The solution left at room temperature to crystallize for 1 h. The resulting crystals were collected and dried under high vacuum for 16 h to afford the title compound as a crystalline solid (21 g, 84%). 1H NMR (400 MHz, DMSO-D6) δ 9.76 (s, 1H) 9.32 (t, 1H) 8.31 (d, 1H) 8.25 (d, 1H) 7.66-7.78 (m, 2H) 7.50-7.65 (m, 3H) 7.39 (q, 1H) 7.23-7.29 (m, 3H) 7.09 (t, 1H) 4.54 (d, 2H).

후처리

  1. customThe title compound was prepared
  2. customThe title compound was further purified
  3. dissolutionby dissolving 25 g in EtOH (300 mL)
  4. temperaturegently heating
  5. customto 80° C
  6. dissolutionThe resulting solids material were then slowly dissolved
  7. additionmore EtOH (50 mL) was added
  8. dissolutionto completely dissolve all the solids
  9. waitThe solution left at room temperature
  10. customto crystallize for 1 h
  11. customThe resulting crystals were collected
  12. customdried under high vacuum for 16 h

출처 및 근거

ORD 기록
ord-e51005026b8440159f1ae8ed703df0c1
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07868026B2

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