Ethanol → Garenoxacin Mesylate

HRID 1018534ノート

反応式

HRID 1018534 の反応式
C([OH:3])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.[CH3:35][S:36]([OH:39])(=[O:38])=[O:37]>O>[OH2:3].[CH3:35][S:36]([OH:39])(=[O:38])=[O:37].[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 6395Methanesulfonic AcidHCID 124093Garenoxacin

生成物 1

HCID 157690Garenoxacin Mesylate

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
40 °C

実験手順

In 192 ml of 50% water-containing ethanol is suspended 24 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 40° C., after which 5.71 g of methanesulfonic 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 thereafter filtered, and the filtrate is concentrated, after which the crystals deposited are collected by filtration to obtain 26.64 g of (R)-1-cyclopropyl-8-difluoromethoxy-7-(1-methyl-2,3-dihydro-1H-5-isoindolyl)-4-oxo-1,4-dihydro-3-quinolinecarboxylic acid methanesulfonate monohydrate.

後処理

  1. customto form a uniform solution
  2. filtrationfiltered
  3. concentrationthe filtrate is concentrated
  4. filtrationafter which the crystals deposited are collected by filtration

出典と根拠

ORDレコード
ord-a1d75f703c4e423ea26e59fa15d2f188
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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