Trifluoroacetic acid → 3-[2-Methyl-4-(3-methyl-4,10-dihydro-3H-2,3,4,9-tetraaza-benzo[f]azulene-9-carbonyl)-phenyl]-propionic Acid

HRID 220865노트

반응식

HRID 220865 반응식
FC(F)(F)C(O)=O.C([O:12][C:13](=[O:40])[CH2:14][CH2:15][C:16]1[CH:21]=[CH:20][C:19]([C:22]([N:24]2[CH2:33][C:32]3[CH:31]=[N:30][N:29]([CH3:34])[C:28]=3[NH:27][C:26]3[CH:35]=[CH:36][CH:37]=[CH:38][C:25]2=3)=[O:23])=[CH:18][C:17]=1[CH3:39])(C)(C)C>ClCCl>[CH3:39][C:17]1[CH:18]=[C:19]([C:22]([N:24]2[CH2:33][C:32]3[CH:31]=[N:30][N:29]([CH3:34])[C:28]=3[NH:27][C:26]3[CH:35]=[CH:36][CH:37]=[CH:38][C:25]2=3)=[O:23])[CH:20]=[CH:21][C:16]=1[CH2:15][CH2:14][C:13]([OH:40])=[O:12]

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 1361283503-[2-Methyl-4-(3-methyl-4,10-dihydro-3H-2,3,4,9-tetraaza-benzo[f]azulene-9-carbonyl)-phenyl]-propionic Acid Tert-butyl Ester

생성물 1

HCID 1361283543-[2-Methyl-4-(3-methyl-4,10-dihydro-3H-2,3,4,9-tetraaza-benzo[f]azulene-9-carbonyl)-phenyl]-propionic Acid수율 90%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Trifluoroacetic acid (5 ml) was added to a solution of 3-[2-methyl-4-(3-methyl-4,10-dihydro-3H-2,3,4,9-tetraaza-benzo[f]azulene-9-carbonyl)-phenyl]-propionic acid tert-butyl ester from Example E45.3 (413 mg, 0.92 mmol) in dichloromethane (10 ml) and the mixture was stirred for 45 min at room temperature. Solvents were removed in vacuo and azeotroped with dichloromethane. The residue was crystallised with MeOH/Et2O to yield the title compound (322 mg, 90%).

후처리

  1. customSolvents were removed in vacuo
  2. customazeotroped with dichloromethane
  3. customThe residue was crystallised with MeOH/Et2O

출처 및 근거

ORD 기록
ord-feef8b707c1a44699b9589db815eabc3
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08202858B2

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