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Acetic Acid → 3-(4-Benzyloxy-phenyl)-3-hydroxy-2-methyl-2-o-tolyloxy-propionic Acid Ethyl Ester

HRID 585280
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HRID 585280 반응식
[Li+].CC([N-]C(C)C)C.[CH2:9]([O:11][C:12](=[O:23])[CH:13]([O:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=1[CH3:22])[CH3:14])[CH3:10].[CH2:24]([O:31][C:32]1[CH:39]=[CH:38][C:35]([CH:36]=[O:37])=[CH:34][CH:33]=1)[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1.C(O)(=O)C.[NH4+].[Cl-]>C1COCC1.C(OCC)C>[CH2:9]([O:11][C:12](=[O:23])[C:13]([CH3:14])([O:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=1[CH3:22])[CH:36]([C:35]1[CH:34]=[CH:33][C:32]([O:31][CH2:24][C:25]2[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=2)=[CH:39][CH:38]=1)[OH:37])[CH3:10]
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참가 물질

8

반응물 5

HCID 176Acetic AcidHCID 25517Ammonium ChlorideHCID 78109Benzaldehyde, 4-(phenylmethoxy)-HCID 2724682Lithium diisopropylamideHCID 10398141Ethyl 2-(2-methylphenoxy)propionate

생성물 1

HCID 208231503-(4-Benzyloxy-phenyl)-3-hydroxy-2-methyl-2-o-tolyloxy-propionic Acid Ethyl Ester
수율 54%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 8028Tetrahydrofuran용매2회

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온도
-78 °C

실험 절차

A solution of LDA (34.9 mL, 52.4 mmol, 1.5M in cyclohexane) in anhydrous THF (60 mL) was cooled to −78° C. in a dry ice/acetone bath and added to a solution of 2-o-Tolyloxy-propionic acid ethyl ester in anhydrous THF (60 mL) also cooled to −78° C. under an atmosphere of nitrogen. After five minutes, 4-benzyloxybenzaldehyde (5.56 g, 26.2 mmol) was added in one portion. After stirring for one minute, the reaction mixture was quenched with acetic acid (5 mL, 87.4 mmol, d=1.049) and a saturated solution of aqueous NH4Cl (50 mL). The biphasic mixture was allowed to warm to room temperature and diluted with diethyl ether (1 L). The organic layer was washed with water, dried over MgSO4, and concentrated in vacuo. The residue was purified by flash column chromatography (13% ethyl acetate in hexanes) to provide a mixture of diastereomers of the titled compound (6.36 g, 54%). 1H NMR (400 MHz, CDCl3): • 7.44-7.32 (m, 6H), 7.16-6.82 (m, 5H), 69.74-6.66 (m, 2H), 5.16 (d, 1H, J=3.52 Hz), 5.07 (s, 2H), 4.26-4.15 (m, 2H), 2.28 (s, 3H), 1.43 (s, 3H), 1.22-1.17 (m, 3H). Rf=0.25 in 25% ethyl acetate in hexanes.

후처리

  1. temperatureto warm to room temperature
  2. washThe organic layer was washed with water
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by flash column chromatography (13% ethyl acetate in hexanes)
  6. customto provide

출처 및 근거

ORD 기록
ord-0fabf10d1f0a4086a617d9c9a3cf89d1
출처 데이터셋
uspto-grants-2005_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06930120B2

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