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

HRID 1985136
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HRID 1985136 반응식
C([O:3][C:4](=[O:43])[C:5]([O:35][C:36]1[CH:41]=[CH:40][CH:39]=[CH:38][C:37]=1[F:42])([CH3:34])[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]=[C:24]([C:28]([F:31])([F:30])[F:29])[CH:23]=3)[C:18](=[O:32])[N:17]2[CH3:33])=[CH:9][CH:8]=1)C.[OH-].[Na+]>C(O)C>[F:42][C:37]1[CH:38]=[CH:39][CH:40]=[CH:41][C:36]=1[O:35][C:5]([CH3:34])([CH2:6][C:7]1[CH:8]=[CH:9][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]=[C:24]([C:28]([F:30])([F:31])[F:29])[CH:23]=3)[C:18](=[O:32])[N:17]2[CH3:33])=[CH:11][CH:12]=1)[C:4]([OH:43])=[O:3]
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참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 68867419HCID 68867419, 화합물

생성물 1

HCID 101966892-(2-Fluoro-phenoxy)-2-methyl-3-(4-{2-[3-methyl-2-oxo-1-(3-trifluoromethyl-benzyl)-imidazolidin-4-yl]-ethoxy}-phenyl)-propionic acid

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of 2-(2-Fluoro-phenoxy)-2-methyl-3-(4-{2-[3-methyl-2-oxo-1-(3-trifluoromethyl-benzyl)-imidazolidin-4-yl]-ethoxy}-phenyl)-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 7.53-7.42 (m, 2H), 7.29-6.93 (m, 7H), 6.85-6.73 (m, 3H), 4.49-4.29 (m, 2H), 3.99-3.95 (m, 2H), 3.81-3.68 (m, 1H), 3.46-3.41 (m, 1H), 3.28, 3.16 (ABq, 2H, J=13.7 Hz), 3.09-3.04 (m, 1H), 2.86 (d, 3H, J=5.6 Hz), 2.25-2.21 (m, 1H), 1.93-1.87 (m, 1H), 1.40 (s, 3H). MS [ES+] m/z exact mass calcd for C30H31N2O5F4 575.2169, found 575.2156.

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-8d38a2689e694a998b50efda288f2782
출처 데이터셋
uspto-grants-2009_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07544812B2

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