Lithium hydroxide, monohydrate → (5-chloro-2-{2-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-2-oxo-ethoxy}-pyridin-3-yl)-acetic acid

HRID 11678노트

반응식

HRID 11678 반응식
C[O:2][C:3](=[O:32])[CH2:4][C:5]1[C:6]([O:12][CH2:13][C:14]([N:16]2[CH2:21][C@H:20]([CH3:22])[N:19]([CH2:23][C:24]3[CH:29]=[CH:28][C:27]([F:30])=[CH:26][CH:25]=3)[CH2:18][C@H:17]2[CH3:31])=[O:15])=[N:7][CH:8]=[C:9]([Cl:11])[CH:10]=1.O.[OH-].[Li+]>O1CCCC1.O>[Cl:11][C:9]1[CH:10]=[C:5]([CH2:4][C:3]([OH:32])=[O:2])[C:6]([O:12][CH2:13][C:14]([N:16]2[CH2:21][C@H:20]([CH3:22])[N:19]([CH2:23][C:24]3[CH:29]=[CH:28][C:27]([F:30])=[CH:26][CH:25]=3)[CH2:18][C@H:17]2[CH3:31])=[O:15])=[N:7][CH:8]=1

참가 물질

5

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 69655283(5-Chloro-2-{2-[4-(4-Fluoro-Benzyl)-(2R,5S)-2,5-Dimethyl-Piperazin-1-Yl]-2-Oxo-Ethoxy}-Pyridin-3-Yl)-Acetic Acid Methyl Ester

생성물 1

HCID 69655717(5-chloro-2-{2-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-2-oxo-ethoxy}-pyridin-3-yl)-acetic acid수율 45.2%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of (5-chloro-2-{2-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-2-oxo-ethoxy}-pyridin-3-yl)-acetic acid methyl ester (0.14 g, 0.3 mmol) in tetrahydrofuran (3.0 mL) and water (0.6 mL) was added lithium hydroxide monohydrate (0.031 g, 0.75 mmol) at ambient temperature. After stirring for 4 hours the reaction mixture was filtered through a pad of silica gel eluting with 10% methanol/dichloromethane. The filtrate was concentrated in vacuo to provide the title compound (0.061 g).

후처리

  1. filtrationwas filtered through a pad of silica gel eluting with 10% methanol/dichloromethane
  2. concentrationThe filtrate was concentrated in vacuo

출처 및 근거

ORD 기록
ord-f3976d1097154f9cbbbd5eda043d05d8
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07098212B2

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