Methanol → HCID 57742533, 화합물

HRID 2266478노트

반응식

HRID 2266478 반응식
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]

참가 물질

6

반응물 4

HCID 887MethanolHCID 962WaterHCID 3939Lithium HydroxideHCID 68783486HCID 68783486, 화합물

생성물 1

HCID 57742533HCID 57742533, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-bf3785d31b914e75b020dd370ae742d4
출처 데이터셋
uspto-grants-2010_12
특허 번호
US07858640B2

반응 노트

불러오는 중…