Ethanol → HCID 68433833、化合物

HRID 1250367ノート

反応式

HRID 1250367 の反応式
C(O)C.[CH:4]1([N:7]2[C:16]3[C:11](=[CH:12][CH:13]=[C:14]([C:21]4[CH:22]=[C:23]5[C:27](=[CH:28][CH:29]=4)[C@@H:26]([CH3:30])[NH:25][CH2:24]5)[C:15]=3[O:17][CH:18]([F:20])[F:19])[C:10](=[O:31])[C:9]([C:32]([OH:34])=[O:33])=[CH:8]2)[CH2:6][CH2:5]1.[S:35](=[O:39])(=[O:38])([OH:37])[OH:36]>O>[S:35]([OH:39])([OH:38])(=[O:37])=[O:36].[CH:4]1([N:7]2[C:16]3[C:11](=[CH:12][CH:13]=[C:14]([C:21]4[CH:22]=[C:23]5[C:27](=[CH:28][CH:29]=4)[C@@H:26]([CH3:30])[NH:25][CH2:24]5)[C:15]=3[O:17][CH:18]([F:20])[F:19])[C:10](=[O:31])[C:9]([C:32]([OH:34])=[O:33])=[CH:8]2)[CH2:6][CH2:5]1

参加物

5

反応物 3

HCID 702EthanolHCID 1118Sulfuric AcidHCID 124093Garenoxacin

生成物 1

HCID 68433833HCID 68433833、化合物収率 55.3%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
50 °C

実験手順

In 10 ml of 50% water-containing ethanol is suspended 0.5 g of (R)-1-cyclopropyl-8-difluoromethoxy-7-(1-methyl-2,3-dihydro-1H-5-isoindolyl)-4-oxo-1,4-dihydro-3-quinolinecarboxylic acid and the suspension is then warmed to 50° C., after which 0.12 g of sulfuric acid is added thereto to form a uniform solution. Subsequently, the solution is stirred at the same temperature for 10 minutes and then filtered. The filtrate is cooled to room temperature and thereafter the crystals deposited are collected by filtration to obtain 0.34 g of (R)-1-cyclopropyl-8-difluoromethoxy-7-(1-methyl-2,3-dihydro-1H-5-isoindolyl)-4-oxo-1,4-dihydro-3-quinolinecarboxylic acid sulfate.

後処理

  1. customto form a uniform solution
  2. filtrationfiltered
  3. temperatureThe filtrate is cooled to room temperature
  4. filtrationthe crystals deposited are collected by filtration

出典と根拠

ORDレコード
ord-f79e6e6039e5473c8e9a2614e52ddc52
出典データセット
uspto-grants-2002_01
特許番号
US06337399B1

反応ノート

読み込み中…