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Acrylamide → 7-[(3RS,5SR)-4-(3-Amino-3-oxopropyl)-3,5-dimethylpiperazin-1-yl]-6-fluoro-8-methoxy-N-[2-methyl-4-(trifluoromethoxy)benzyl]-4-oxo-1-(2,2,2-trifluoroethyl)-1,4-dihydroquinoline-3-carboxamide

HRID 251864
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인쇄 미리보기

반응식

HRID 251864 반응식
[CH3:1][CH:2]1[NH:7][CH:6]([CH3:8])[CH2:5][N:4]([C:9]2[C:18]([O:19][CH3:20])=[C:17]3[C:12]([C:13](=[O:42])[C:14]([C:26]([NH:28][CH2:29][C:30]4[CH:35]=[CH:34][C:33]([O:36][C:37]([F:40])([F:39])[F:38])=[CH:32][C:31]=4[CH3:41])=[O:27])=[CH:15][N:16]3[CH2:21][C:22]([F:25])([F:24])[F:23])=[CH:11][C:10]=2[F:43])[CH2:3]1.[C:44]([NH2:48])(=[O:47])[CH:45]=[CH2:46].Cl([O-])(=O)(=O)=O.[Li+]>C(#N)C.CS(C)=O>[NH2:48][C:44](=[O:47])[CH2:45][CH2:46][N:7]1[CH:6]([CH3:8])[CH2:5][N:4]([C:9]2[C:18]([O:19][CH3:20])=[C:17]3[C:12]([C:13](=[O:42])[C:14]([C:26]([NH:28][CH2:29][C:30]4[CH:35]=[CH:34][C:33]([O:36][C:37]([F:40])([F:38])[F:39])=[CH:32][C:31]=4[CH3:41])=[O:27])=[CH:15][N:16]3[CH2:21][C:22]([F:25])([F:24])[F:23])=[CH:11][C:10]=2[F:43])[CH2:3][CH:2]1[CH3:1]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 6579AcrylamideHCID 23665649Lithium perchlorateHCID 724938447-[(3RS,5SR)-3,5-Dimethylpiperazin-1-yl]-6-fluoro-8-methoxy-N-[2-methyl-4-(trifluoromethoxy)benzyl]-4-oxo-1-(2,2,2-trifluoroethyl)-1,4-dihydroquinoline-3-carboxamide

생성물 1

HCID 724938167-[(3RS,5SR)-4-(3-Amino-3-oxopropyl)-3,5-dimethylpiperazin-1-yl]-6-fluoro-8-methoxy-N-[2-methyl-4-(trifluoromethoxy)benzyl]-4-oxo-1-(2,2,2-trifluoroethyl)-1,4-dihydroquinoline-3-carboxamide

시약·촉매·용매 2

HCID 6342Acetonitrile촉매HCID 679Dimethyl Sulfoxide용매

반응 조건

온도
70 °C

실험 절차

A few drops of acetonitrile are added at room temperature to 55 mg of the compound of Example 52, 18 mg of acrylamide and 35 mg of lithium perchlorate, so that a stirrable suspension results. The mixture is heated to 70° C. over night and left to cool. After the addition of DMSO the whole mixture is separated by preparative HPLC (Method 5). After concentrating the suitable fractions and drying under high vacuum 30 mg (40% of theory) of the title compound are obtained.

후처리

  1. customresults
  2. waitleft
  3. temperatureto cool
  4. customis separated by preparative HPLC (Method 5)
  5. concentrationAfter concentrating the suitable fractions
  6. dry with materialdrying under high vacuum 30 mg (40% of theory) of the title compound
  7. customare obtained

출처 및 근거

ORD 기록
ord-0b93aa94662c4e62b1e0a9feeacf9e77
출처 데이터셋
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07867992B2

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