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Sodium Hydroxide → 3-{4-[2-(1-Benzyl-3-methyl-2-oxo-imidazolidin-4-yl)-ethoxy]-phenyl}-2-(2-fluoro-phenoxy)-2-methyl-propionic acid

HRID 1985132
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HRID 1985132 반응식
C([O:3][C:4](=[O:39])[C:5]([O:31][C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][C:33]=1[F:38])([CH3:30])[CH2:6][C:7]1[CH:12]=[CH:11][C:10]([O:13][CH2:14][CH2:15][CH:16]2[CH2:20][N:19]([CH2:21][C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[C:18](=[O:28])[N:17]2[CH3:29])=[CH:9][CH:8]=1)C.[OH-].[Na+]>C(O)C>[CH2:21]([N:19]1[CH2:20][CH:16]([CH2:15][CH2:14][O:13][C:10]2[CH:11]=[CH:12][C:7]([CH2:6][C:5]([O:31][C:32]3[CH:37]=[CH:36][CH:35]=[CH:34][C:33]=3[F:38])([CH3:30])[C:4]([OH:39])=[O:3])=[CH:8][CH:9]=2)[N:17]([CH3:29])[C:18]1=[O:28])[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 68867323HCID 68867323, 화합물

생성물 1

HCID 102891963-{4-[2-(1-Benzyl-3-methyl-2-oxo-imidazolidin-4-yl)-ethoxy]-phenyl}-2-(2-fluoro-phenoxy)-2-methyl-propionic acid

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of 3-{4-[2-(1-Benzyl-3-methyl-2-oxo-imidazolidin-4-yl)-ethoxy]-phenyl}-2-(2-fluoro-phenoxy)-2-methyl-propionic acid ethyl ester and 5N NaOH (0.2 mL) in ethanol (2 mL) is refluxed under nitrogen for 1 h, cooled to ambient temperature, and concentrated in vacuo. The residue is diluted with 1N HCl, extracted with CH2Cl2, dried, concentrated in vacuo, and purified by LCMS to provide the title compound. 1H NMR (400 MHz, CDCl3): δ 7.55 (d, 1H, J=8.4 Hz), 7.34-7.21 (m, 6H), 7.10-7.01 (m, 4H), 6.74 (d, 2H, J=8.4 Hz), 4.46-3.36 (m, 2H), 3.96 (q, 2H, J=6.0 Hz), 3.74-3.65 (m, 1H), 3.45-3.39 (m, 1H), 3.28, 3.16 (ABq, 2H, J=14.7 Hz), 3.05 (q, 1H, J=8.6 Hz), 2.26-2.19 (m, 1H), 1.93-1.86 (m, 1H), 1.41 (s, 3H). MS [EI+] 507 (M+H)+.

후처리

  1. concentrationconcentrated in vacuo
  2. additionThe residue is diluted with 1N HCl
  3. extractionextracted with CH2Cl2
  4. customdried
  5. concentrationconcentrated in vacuo
  6. custompurified by LCMS

출처 및 근거

ORD 기록
ord-a5d3643446a04236b3fe96407a38b934
출처 데이터셋
uspto-grants-2009_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07544812B2

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