Ethanol → HCID 68431852、化合物

HRID 1018537ノート

反応式

HRID 1018537 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.[P:35](=[O:39])([OH:38])([OH:37])[OH:36]>O>[P:35]([OH:39])([OH:38])([OH: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 1004Phosphoric AcidHCID 124093Garenoxacin

生成物 1

HCID 68431852HCID 68431852、化合物収率 52%

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 warmed to 50° C., after which 0.14 g of phosphoric acid is added to the warmed suspension to form a uniform solution. Subsequently, the solution is stirred at the same temperature for 10 minutes and then subjected to filtration. The filtrate is cooled to room temperature and then the crystals deposited are collected by filtration to obtain 0.32 g of (R)-1-cyclopropyl-8-difluoromethoxy-7-(1-methyl-2,3-dihydro-1H-5-isoindolyl)-4-oxo-1,4-dihydro-3-quinolinecarboxylic acid phosphate.

後処理

  1. customto form a uniform solution
  2. filtrationsubjected to filtration
  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-bee5593e633f4c81ad0c68fe951f40e4
出典データセット
uspto-grants-2002_11
特許番号
US06482835B2

反応ノート

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