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Sodium hydride → HCID 68867419, 화합물

HRID 1985145
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HRID 1985145 반응식
[F:1][C:2]([F:12])([F:11])[C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][CH:10]=1)[CH2:6]Br.[CH2:13]([O:15][C:16](=[O:44])[C:17]([O:36][C:37]1[CH:42]=[CH:41][CH:40]=[CH:39][C:38]=1[F:43])([CH3:35])[CH2:18][C:19]1[CH:24]=[CH:23][C:22]([O:25][CH2:26][CH2:27][CH:28]2[CH2:32][NH:31][C:30](=[O:33])[N:29]2[CH3:34])=[CH:21][CH:20]=1)[CH3:14].[H-].[Na+]>[I-].C([N+](CCCC)(CCCC)CCCC)CCC.C(OCC)(=O)C>[CH2:13]([O:15][C:16](=[O:44])[C:17]([O:36][C:37]1[CH:42]=[CH:41][CH:40]=[CH:39][C:38]=1[F:43])([CH3:35])[CH2:18][C:19]1[CH:24]=[CH:23][C:22]([O:25][CH2:26][CH2:27][CH:28]2[CH2:32][N:31]([CH2:6][C:5]3[CH:8]=[CH:9][CH:10]=[C:3]([C:2]([F:12])([F:11])[F:1])[CH:4]=3)[C:30](=[O:33])[N:29]2[CH3:34])=[CH:21][CH:20]=1)[CH3:14]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 24758Sodium hydrideHCID 1230611-(Bromomethyl)-3-(trifluoromethyl)benzeneHCID 68867329HCID 68867329, 화합물

생성물 1

HCID 68867419HCID 68867419, 화합물

시약·촉매·용매 2

HCID 67553Tetrabutylammonium Iodide촉매HCID 8857Ethyl Acetate
용매

실험 절차

3-Trifluoromethylbenzyl bromide (0.03 mL, 0.165 mmol, d=1.565) and tetrabutyl ammonium iodide (catalytic amount) are added to a 0° C. suspension of 2-(2-Fluoro-phenoxy)-2-methyl-3-{4-[2-(3-methyl-2-oxo-imidazolidin-4-yl)-ethoxy]-phenyl}-propionic acid ethyl ester (0.049 g, 0.110 mmol) and sodium hydride (0.011 g, 0.276 mmol, 60% suspension on mineral oil), pre-stirred for 1 h at ambient temperature. The reaction mixture is stirred at ambient temperature for 18 h, diluted with ethyl acetate, and washed. The organic layer is dried, concentrated, and carried into the next step. MS [EI+] 603 (M+H)+.

후처리

  1. stirringThe reaction mixture is stirred at ambient temperature for 18 h
  2. washwashed
  3. customThe organic layer is dried
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-725966bc793e45faa529c522824fbc79
출처 데이터셋
uspto-grants-2009_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07544812B2

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