Dimethylformamide → 1-(3-amino-4,6-difluorophenyl)-7-[(3S)-3-aminopyrrolidin-1-yl]-6-fluoro-1,4-dihydro-4-oxo-1,8-naphthyridine-3-carboxylic acid

HRID 1415938

反応式

HRID 1415938 の反応式
CN(C)C=O.[NH2:6][C:7]1[CH:8]=[C:9]([N:15]2[C:24]3[C:19](=[CH:20][C:21]([F:26])=[C:22](Cl)[N:23]=3)[C:18](=[O:27])[C:17]([C:28]([OH:30])=[O:29])=[CH:16]2)[C:10]([F:14])=[CH:11][C:12]=1[F:13].[NH2:31][C@H:32]1[CH2:36][CH2:35][NH:34][CH2:33]1.C(N(CC)CC)C>C(O)C>[CH:32]([O:27][CH:18]([CH3:17])[CH3:19])([CH3:36])[CH3:33].[NH2:6][C:7]1[CH:8]=[C:9]([N:15]2[C:24]3[C:19](=[CH:20][C:21]([F:26])=[C:22]([N:34]4[CH2:35][CH2:36][C@H:32]([NH2:31])[CH2:33]4)[N:23]=3)[C:18](=[O:27])[C:17]([C:28]([OH:30])=[O:29])=[CH:16]2)[C:10]([F:14])=[CH:11][C:12]=1[F:13]

参加物

7

反応条件

温度
90 °C

実験手順

To 6,500 mg of N,N-dimethylformamide were added 1,300 mg of 1-(3-amino-4,6-difluorophenyl)-7-chloro-6-fluoro-4-oxo-1,4-dihydro-1,8-naphthyridine-3-carboxylic acid, 600 mg of (3S)-3-aminopyrrolidine, and 1,000 mg of triethylamine. The solution was stirred at 90° C. for 1 hour. The reaction solution was allowed to cool down, combined with 25 ml of ethanol, heated at reflux for 5 minutes, and allowed to cool down. The precipitate was collected by filtration and washed with ethanol and then with diisopropyl ether to give 1,410 mg of the title compound.

後処理

  1. temperatureto cool down
  2. temperatureheated
  3. temperatureat reflux for 5 minutes
  4. temperatureto cool down
  5. filtrationThe precipitate was collected by filtration
  6. washwashed with ethanol

出典と根拠

ORDレコード
ord-b023eee62d134e96bb708fa16541416f
出典データセット
uspto-grants-1999_06
特許番号
US05910498

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