Methanesulfonic Acid → Garenoxacin Mesylate

HRID 1250358ノート

反応式

HRID 1250358 の反応式
O.[CH:2]1([N:5]2[C:14]3[C:9](=[CH:10][CH:11]=[C:12]([C:19]4[CH:20]=[C:21]5[C:25](=[CH:26][CH:27]=4)[C@@H:24]([CH3:28])[NH:23][CH2:22]5)[C:13]=3[O:15][CH:16]([F:18])[F:17])[C:8](=[O:29])[C:7]([C:30]([OH:32])=[O:31])=[CH:6]2)[CH2:4][CH2:3]1.[CH3:33][S:34]([OH:37])(=[O:36])=[O:35]>C(O)C>[OH2:15].[CH3:33][S:34]([OH:37])(=[O:36])=[O:35].[CH:2]1([N:5]2[C:14]3[C:9](=[CH:10][CH:11]=[C:12]([C:19]4[CH:20]=[C:21]5[C:25](=[CH:26][CH:27]=4)[C@@H:24]([CH3:28])[NH:23][CH2:22]5)[C:13]=3[O:15][CH:16]([F:18])[F:17])[C:8](=[O:29])[C:7]([C:30]([OH:32])=[O:31])=[CH:6]2)[CH2:4][CH2:3]1

参加物

4

反応物 2

HCID 6395Methanesulfonic AcidHCID 68432514HCID 68432514、化合物

生成物 1

HCID 157690Garenoxacin Mesylate収率 182.5%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
40 °C

実験手順

In 192 ml of 50% 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 monohydrate, and the suspension is warmed to 40° C., after which 5.71 g of methanesulfonic acid is added to form a uniform solution. Subsequently, 2.4 g of activated carbon is added and the resulting mixture is stirred at the same temperature for 10 minutes, after which the insolubles are removed by filtration. The filtrate is concentrated and 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. additionSubsequently, 2.4 g of activated carbon is added
  3. customafter which the insolubles are removed by filtration
  4. concentrationThe filtrate is concentrated
  5. filtrationthe crystals deposited are collected by filtration

出典と根拠

ORDレコード
ord-53f26a2272544d19840de385007015a3
出典データセット
uspto-grants-2002_01
特許番号
US06337399B1

反応ノート

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