HCID 86704966, 화합물 → HCID 68350583, 화합물

HRID 572154노트

반응식

HRID 572154 반응식
[CH3:1][C:2]1[N:3]=[C:4]2[C:9]([C:10]3[CH:33]=[CH:32][C:13]([O:14][C:15]4[N:19](COCC[Si](C)(C)C)[C:18]5[CH:28]=[CH:29][CH:30]=[CH:31][C:17]=5[N:16]=4)=[CH:12][CH:11]=3)=[CH:8][CH:7]=[CH:6][N:5]2[CH:34]=1>C(OCC)(=O)C.Cl>[CH3:1][C:2]1[N:3]=[C:4]2[C:9]([C:10]3[CH:33]=[CH:32][C:13]([O:14][C:15]4[NH:19][C:18]5[CH:28]=[CH:29][CH:30]=[CH:31][C:17]=5[N:16]=4)=[CH:12][CH:11]=3)=[CH:8][CH:7]=[CH:6][N:5]2[CH:34]=1

참가 물질

3

반응물 1

HCID 86704966HCID 86704966, 화합물

생성물 1

HCID 68350583HCID 68350583, 화합물수율 84.9%

시약·촉매·용매 1

HCID 21866389Hydrogen chloride-ethyl acetate용매

실험 절차

A mixture of 2-[4-(2-methylimidazo[1,2-a]pyridin-8-yl)phenoxy]-1-{[2-(trimethylsilyl)ethoxy]methyl}-1H-benzimidazole (0.57 g) and 4 M hydrogen chloride-ethyl acetate solution (20 ml) was heated under reflux for 3 hr. The reaction mixture was concentrated under reduced pressure, saturated aqueous sodium hydrogen carbonate solution was added to the residue, and the mixture was extracted with ethyl acetate. The extract was dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was recrystallized from ethyl acetate to give the title compound (0.35 g).

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 3 hr
  3. concentrationThe reaction mixture was concentrated under reduced pressure, saturated aqueous sodium hydrogen carbonate solution
  4. additionwas added to the residue
  5. extractionthe mixture was extracted with ethyl acetate
  6. dry with materialThe extract was dried over anhydrous sodium sulfate
  7. customthe solvent was evaporated under reduced pressure
  8. customThe residue was recrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-4245c6d26e4d4a83b69b62e6fba5590c
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09029388B2

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