Pyridine → HCID 22935750, 화합물

HRID 1352505노트

반응식

HRID 1352505 반응식
C(OC(=O)C)(=[O:3])C.C1(N[C:12]2[C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[N:15]=[CH:14][CH:13]=2)CC1.[N:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1>>[CH:25]1([CH:26]([C:12]2[C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[N:15]=[CH:14][CH:13]=2)[C:27]([NH2:22])=[O:3])[CH2:23][CH2:24]1

참가 물질

4

반응물 3

HCID 1049PyridineHCID 7918Acetic AnhydrideHCID 22935736681828-34-2

생성물 1

HCID 22935750HCID 22935750, 화합물수율 98.7%

실험 절차

Acetic anhydride (18.3 g) was added to a solution of cyclopropyl-quinolin-4-yl-amine (6.6 g) in pyridine (50 ml) and the mixture was heated under reflux over night. After cooling, the solvent was removed under reduce pressure and then the mixture was washed with dichloromethane (200 ml) and an aqueous solution of sodium carbonate (200 ml). The organic layer was separated and dried over sodium sulfate. The solvent was removed under reduce pressure and the crude compound was purified by flash chromatography on silicagel using dichloromethane/methanol (98/2) as eluent to give cyclopropyl-quinolin-4-yl-acetamide (8 g, 98.7% yield).

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux over night
  3. temperatureAfter cooling
  4. customthe solvent was removed
  5. washthe mixture was washed with dichloromethane (200 ml)
  6. customThe organic layer was separated
  7. dry with materialdried over sodium sulfate
  8. customThe solvent was removed
  9. customthe crude compound was purified by flash chromatography on silicagel

출처 및 근거

ORD 기록
ord-89eb4b1c909f4499bbe1ad59f0cace37
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07220760B2

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