Methanol → Methyl 4-[4-(4-fluorophenyl)-5-(4-pyridyl)-1H-imidazol-2-yl]-benzoate

HRID 2293492노트

반응식

HRID 2293492 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:9]=[C:10]([C:19]3[CH:27]=[CH:26][C:22]([C:23]([OH:25])=[O:24])=[CH:21][CH:20]=3)[NH:11][C:12]=2[C:13]2[CH:18]=[CH:17][N:16]=[CH:15][CH:14]=2)=[CH:4][CH:3]=1.[Na].[OH-].[Na+].[CH3:31]O>Cl>[F:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[N:9]=[C:10]([C:19]3[CH:27]=[CH:26][C:22]([C:23]([O:25][CH3:31])=[O:24])=[CH:21][CH:20]=3)[NH:11][C:12]=2[C:13]2[CH:18]=[CH:17][N:16]=[CH:15][CH:14]=2)=[CH:6][CH:7]=1

참가 물질

6

반응물 4

HCID 887MethanolHCID 14798Sodium HydroxideHCID 5360545SodiumHCID 110574684-[4-(4-fluorophenyl)-5-(4-pyridyl)-1H-imidazol-2-yl]benzoic acid

생성물 1

HCID 10133915Methyl 4-[4-(4-fluorophenyl)-5-(4-pyridyl)-1H-imidazol-2-yl]-benzoate

시약·촉매·용매 1

HCID 313Hydrochloric Acid촉매

실험 절차

A mixture containing 4-[4-(4-fluorophenyl)-5-(4-pyridyl)-1H-imidazol-2-yl]benzoic acid, sodium salt (0.20 g, 0.5 mmol) [See Ex. 9 above] and concentrated HCl (10 drops) in MeOH (5 mL) was heated at reflux for 8 h. After cooling, the pH was adjusted to neutral by the addition of 2.5N NaOH, and the solid which formed was collected by filtration, washed with H2O and dried in vacuo. The title compound was obtained as a yellow solid (0.14 g, 76%) and was recrystallized from EtOAc/CH2Cl2 : 1H NMR (CDCl3 /MeOH-d4): δ8.36 (d, 2H); 8.03 (m, 4H); 7.60-7.30 (m, 4H); 7.07 (t, 2H); 3.84 (s,3H).

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 8 h
  3. temperatureAfter cooling
  4. customthe solid which formed
  5. filtrationwas collected by filtration
  6. washwashed with H2O
  7. customdried in vacuo

출처 및 근거

ORD 기록
ord-e19110aa399f437686dab41aeb5e0b08
출처 데이터셋
uspto-grants-1997_11
특허 번호
US05686455

반응 노트

불러오는 중…