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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
ノート
印刷プレビュー

反応式

HRID 251864 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 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

生成物 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

試薬・触媒・溶媒 2

HCID 6342Acetonitrile触媒HCID 679Dimethyl Sulfoxide溶媒

反応条件

温度
70 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0b93aa94662c4e62b1e0a9feeacf9e77
出典データセット
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07867992B2

反応ノート

読み込み中…

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