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Methanol → [8-Chloro-3-(4-chlorobenzyl)-4-methoxy-2-methylquinolin-5-yloxy]acetic acid

HRID 2266420
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HRID 2266420 반응식
C[O:2][C:3](=[O:28])[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][CH3:27])=[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:28])=[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][CH3:27]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 887MethanolHCID 3939Lithium HydroxideHCID 68781739HCID 68781739, 화합물

생성물 1

HCID 57742487[8-Chloro-3-(4-chlorobenzyl)-4-methoxy-2-methylquinolin-5-yloxy]acetic acid

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of [8-chloro-3-(4-chlorobenzyl)-4-methoxy-2-methylquinolin-5-yloxy]acetic acid methyl ester (0.059 g), methanol (2.0 mL), saturated aqueous lithium hydroxide solution (0.25 mL) and water (0.4 mL) was stirred at room temperature for 15 hours, The methanol was removed under reduced pressure and the pH of the residue adjusted to 1 by the addition of 1.0 M aqueous hydrochloric acid. Purification by preparative reverse-phase HPLC using a gradient over 30 minutes of acetonitrile in water (20% to 80% of organic modifier) gave title compound as a yellow solid, 0.060 g.

후처리

  1. customThe methanol was removed under reduced pressure
  2. additionthe pH of the residue adjusted to 1 by the addition of 1.0 M aqueous hydrochloric acid
  3. customPurification by preparative reverse-phase
  4. customover 30 minutes

출처 및 근거

ORD 기록
ord-de7d44cdc45540b584fd0780b03a0ebe
출처 데이터셋
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07858640B2

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