Lithium Hydroxide → HCID 16660416, 화합물

HRID 2266629노트

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HRID 2266629 반응식
C[O:2][C:3](=[O:38])[CH2:4][O:5][C:6]1[CH:15]=[CH:14][C:13]([F:16])=[C:12]2[C:7]=1[C:8]([O:34][CH:35]([F:37])[F:36])=[C:9]([CH2:19][C:20]1[CH:25]=[CH:24][C:23]([C:26](=[O:32])[NH:27][CH:28]3[CH2:31][CH2:30][CH2:29]3)=[CH:22][C:21]=1[Cl:33])[C:10]([CH2:17][CH3:18])=[N:11]2.[OH-].[Li+]>O1CCCC1>[Cl:33][C:21]1[CH:22]=[C:23]([C:26](=[O:32])[NH:27][CH:28]2[CH2:31][CH2:30][CH2:29]2)[CH:24]=[CH:25][C:20]=1[CH2:19][C:9]1[C:10]([CH2:17][CH3:18])=[N:11][C:12]2[C:7]([C:8]=1[O:34][CH:35]([F:37])[F:36])=[C:6]([O:5][CH2:4][C:3]([OH:38])=[O:2])[CH:15]=[CH:14][C:13]=2[F:16]

참가 물질

4

반응물 2

HCID 3939Lithium HydroxideHCID 68784786HCID 68784786, 화합물

생성물 1

HCID 16660416HCID 16660416, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of [3-(2-chloro-4-cyclobutylcarbamoylbenzyl)-4-difluoromethoxy-2-ethyl-8-fluoroquinolin-5-yloxy]acetic acid methyl ester (0.23 g), tetrahydrofuran (5.0 mL) and 1.0 M aqueous lithium hydroxide solution (1.2 mL) was stirred at room temperature for 30 minutes. The mixture was concentrated under reduced pressure, acidified by the addition of sodium dihydrogenphosphate and extracted with ethyl acetate. The combined extracts were dried over magnesium sulfate and the solvent removed under reduced pressure. Purification of the residue by column chromatography on C-18 column, eluting with a mixture of water and methanol gave title compound as an off-white solid, 0.13 g.

후처리

  1. concentrationThe mixture was concentrated under reduced pressure
  2. additionacidified by the addition of sodium dihydrogenphosphate
  3. extractionextracted with ethyl acetate
  4. dry with materialThe combined extracts were dried over magnesium sulfate
  5. customthe solvent removed under reduced pressure
  6. customPurification of the residue by column chromatography on C-18 column
  7. washeluting with a mixture of water and methanol

출처 및 근거

ORD 기록
ord-5d847f0bf76845679e5e592c8df0de16
출처 데이터셋
uspto-grants-2010_12
특허 번호
US07858640B2

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