Methanol → HCID 57742533、化合物

HRID 2266478ノート

反応式

HRID 2266478 の反応式
C[O:2][C:3](=[O:33])[CH2:4][O:5][C:6]1[CH:15]=[CH:14][C:13]([Cl:16])=[C:12]2[C:7]=1[C:8]([O:29][CH:30]([F:32])[F:31])=[C:9]([CH2:18][C:19]1[CH:24]=[CH:23][C:22]([S:25]([CH3:28])(=[O:27])=[O:26])=[CH:21][CH:20]=1)[C:10]([CH3:17])=[N:11]2.CO.[OH-].[Li+].O>C(O)(=O)C>[Cl:16][C:13]1[CH:14]=[CH:15][C:6]([O:5][CH2:4][C:3]([OH:33])=[O:2])=[C:7]2[C:12]=1[N:11]=[C:10]([CH3:17])[C:9]([CH2:18][C:19]1[CH:20]=[CH:21][C:22]([S:25]([CH3:28])(=[O:26])=[O:27])=[CH:23][CH:24]=1)=[C:8]2[O:29][CH:30]([F:31])[F:32]

参加物

6

反応物 4

HCID 887MethanolHCID 962WaterHCID 3939Lithium HydroxideHCID 68783486HCID 68783486、化合物

生成物 1

HCID 57742533HCID 57742533、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A solution of [8-chloro-4-difluoromethoxy-3-(4-methanesulfonylbenzyl)-2-methylquinolin-5-yloxy]acetic acid methyl ester (0.13 g), methanol (20 mL), saturated, aqueous lithium hydroxide solution (1.0 mL) and water (2.0 mL) was stirred at room temperature for 45 minutes. The pH of the solution was adjusted to 5 by the addition of glacial acetic acid and the methanol removed under reduced pressured. The resulting precipitate was collected by filtration and purified by preparative reverse-phase HPLC using a gradient over 45 minutes of acetonitrile in water (10% to 95% of organic modifier) to afford title compound as a pale yellow solid, 0.014 g.

後処理

  1. customthe methanol removed
  2. filtrationThe resulting precipitate was collected by filtration
  3. custompurified by preparative reverse-phase
  4. customover 45 minutes

出典と根拠

ORDレコード
ord-bf3785d31b914e75b020dd370ae742d4
出典データセット
uspto-grants-2010_12
特許番号
US07858640B2

反応ノート

読み込み中…