Methanol → HCID 57742523, 화합물

HRID 2266443노트

반응식

HRID 2266443 반응식
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]

참가 물질

5

반응물 3

HCID 887MethanolHCID 3939Lithium HydroxideHCID 68780083HCID 68780083, 화합물

생성물 1

HCID 57742523HCID 57742523, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7f85c234be7140ad89b12f229eef0173
출처 데이터셋
uspto-grants-2010_12
특허 번호
US07858640B2

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