Trifluoroacetic acid → Ethyl 1-(6-amino-3,5-difluoropyridin-2-yl)-5-benzylamino-6,7,8-trifluoro-4-oxo-1,4-dihydroquinoline-3-carboxylate

HRID 368502노트

반응식

HRID 368502 반응식
[CH2:1]([NH:8][C:9]1[C:18]([F:19])=[C:17]([F:20])[C:16]([F:21])=[C:15]2[C:10]=1[C:11](=[O:45])[C:12]([C:40]([O:42][CH2:43][CH3:44])=[O:41])=[CH:13][N:14]2[C:22]1[C:27]([F:28])=[CH:26][C:25]([F:29])=[C:24]([NH:30]CC2C=CC(OC)=CC=2)[N:23]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.FC(F)(F)C(O)=O>>[NH2:30][C:24]1[N:23]=[C:22]([N:14]2[C:15]3[C:10](=[C:9]([NH:8][CH2:1][C:2]4[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=4)[C:18]([F:19])=[C:17]([F:20])[C:16]=3[F:21])[C:11](=[O:45])[C:12]([C:40]([O:42][CH2:43][CH3:44])=[O:41])=[CH:13]2)[C:27]([F:28])=[CH:26][C:25]=1[F:29]

참가 물질

3

반응물 2

HCID 6422Trifluoroacetic acidHCID 22121197Ethyl 5-benzylamino-1-[3,5-difluoro-6-(p-methoxybenzylamino)pyridin-2-yl]-6,7,8-trifluoro-4-oxo-1,4-dihydroquinoline-3-carboxylate

생성물 1

HCID 22121167Ethyl 1-(6-amino-3,5-difluoropyridin-2-yl)-5-benzylamino-6,7,8-trifluoro-4-oxo-1,4-dihydroquinoline-3-carboxylate수율 109.4%

실험 절차

To 600 mg of ethyl 5-benzylamino-1-[3,5-difluoro-6-(p-methoxybenzylamino)pyridine-2-yl]-6,7,8-trifluoro-4-oxo-1,4-dihydroquinoline-3-carboxylate was added 2 ml of trifluoroacetic acid, and the mixture was allowed to stand at room temperature for 20 minutes. The solution was concentrated under reduced pressure, and 3 ml of ethanol was added to the residue, and the solution was again concentrated under reduced pressure. The precipitate was dispersed in ethanol, collected by filtration and washed with ethanol to obtain 530 mg of the title compound as a yellow powder.

후처리

  1. concentrationThe solution was concentrated under reduced pressure, and 3 ml of ethanol
  2. additionwas added to the residue
  3. concentrationthe solution was again concentrated under reduced pressure
  4. additionThe precipitate was dispersed in ethanol
  5. filtrationcollected by filtration
  6. washwashed with ethanol

출처 및 근거

ORD 기록
ord-61aca189716541788770a913cf375a5a
출처 데이터셋
uspto-grants-2000_10
특허 번호
US06133284

반응 노트

불러오는 중…