Methanol → HCID 57742523、化合物

HRID 2266443ノート

反応式

HRID 2266443 の反応式
C[O:2][C:3](=[O:30])[CH2:4][O:5][C:6]1[CH:15]=[CH:14][C:13]([Cl:16])=[C:12]2[C:7]=1[C:8]([O:26][CH:27]([F:29])[F:28])=[C:9]([CH2:18][C:19]1[CH:24]=[CH:23][C:22]([Cl:25])=[CH:21][CH:20]=1)[C:10]([CH3:17])=[N:11]2.CO.[OH-].[Li+]>O>[Cl:16][C:13]1[CH:14]=[CH:15][C:6]([O:5][CH2:4][C:3]([OH:30])=[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]([Cl:25])=[CH:23][CH:24]=1)=[C:8]2[O:26][CH:27]([F:29])[F:28]

参加物

5

反応物 3

HCID 887MethanolHCID 3939Lithium HydroxideHCID 68780083HCID 68780083、化合物

生成物 1

HCID 57742523HCID 57742523、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of [8-chloro-3-(4-chlorobenzyl)-4-difluoromethoxy-2-methylquinolin-5-yloxy]acetic acid methyl ester (0.10 g), methanol (6.0 mL), water (0.6 mL) and saturated aqueous lithium hydroxide solution (0.3 mL) was stirred at room temperature for 17 hours. The methanol was removed under reduced pressure and the pH of the residue adjusted to 4 by the addition of glacial acetic acid. The resulting precipitate was collected by filtration and washed with water. Purification of the solid by preparative reverse-phase HPLC using a gradient over 37 minutes of acetonitrile in water (20% to 95% of organic modifier) gave title compound as a cream solid, 0.020 g.

後処理

  1. customThe methanol was removed under reduced pressure
  2. additionthe pH of the residue adjusted to 4 by the addition of glacial acetic acid
  3. filtrationThe resulting precipitate was collected by filtration
  4. washwashed with water
  5. customPurification of the solid by preparative reverse-phase
  6. customover 37 minutes

出典と根拠

ORDレコード
ord-7f85c234be7140ad89b12f229eef0173
出典データセット
uspto-grants-2010_12
特許番号
US07858640B2

反応ノート

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