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Diethyl Ether → 1-(4-Methoxyphenyl)-2-phenyl-1-(4-pivaloyloxyphenyl)-3-butene

HRID 1926574
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HRID 1926574 반응식
[C:1]([O:7][C:8]1[CH:15]=[CH:14][C:11]([CH:12]=O)=[CH:10][CH:9]=1)(=[O:6])[C:2]([CH3:5])([CH3:4])[CH3:3].C[Si](C)(C)[CH2:18][CH:19]=[CH:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.O.C(=O)(O)[O-].[Na+].[CH2:35]([O:37][CH2:38][CH3:39])C>C1(OC)C=CC=CC=1.[Cl-].[Hf+4].[Cl-].[Cl-].[Cl-]>[CH3:35][O:37][C:38]1[CH:39]=[CH:10][C:9]([CH:12]([C:11]2[CH:14]=[CH:15][C:8]([O:7][C:1](=[O:6])[C:2]([CH3:5])([CH3:4])[CH3:3])=[CH:9][CH:10]=2)[CH:20]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[CH:19]=[CH2:18])=[CH:8][CH:15]=1
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참가 물질

7

반응물 4

HCID 3283Diethyl EtherHCID 142474CinnamyltrimethylsilaneHCID 146834134-Formylphenyl 2,2-dimethylpropanoateHCID 86585896Sodium bicarbonate water

생성물 1

HCID 251119881-(4-Methoxyphenyl)-2-phenyl-1-(4-pivaloyloxyphenyl)-3-butene수율 75%

시약·촉매·용매 2

HCID 9927068
Hafnium chloride (HfCl4) (6CI,8CI); Hafnium chloride; Hafnium tetrachloride; Hafnium(IV) chloride; Hafnium chloride (HfCl4), (T-4)-
촉매
HCID 7519Anisole용매2회

실험 절차

Under an argon atmosphere, hafnium chloride (39.2 mg, 0.122 mmol) is suspended in anisole (3, 0.02 mL), and under ice cooling, an anisole (0.22 mL) solution of 4-(pivaloyloxy)benzaldehyde (1, 25 mg, 0.121 mmol) and trimethylcinnamylsilane (2, 46.7 mg, 0.245 mmol) was slowly added dropwise. After stirring overnight at room temperature, saturated sodium bicarbonate water (5 mL) was poured into the reaction mixture with vigorous stirring, diethyl ether (10 mL) was added and extraction was performed. Extractions were further carried out two times with diethyl ether (10 mL), the organic layers were combined, washed with a saturated sodium chloride aqueous solution (5 mL), dried with anhydrous magnesium sulfate, and concentrated. The residue was purified by thin layer chromatography (hexane:methylene chloride:diethyl ether=4:1:1), and the subject compound (4, 37.7 mg) was obtained as a colorless oily substance (yield 75%, syn/anti mixture).

후처리

  1. additionwas added
  2. extractionextraction
  3. extractionExtractions
  4. washwashed with a saturated sodium chloride aqueous solution (5 mL)
  5. dry with materialdried with anhydrous magnesium sulfate
  6. concentrationconcentrated
  7. customThe residue was purified by thin layer chromatography (hexane:methylene chloride:diethyl ether=4:1:1)
  8. customthe subject compound (4, 37.7 mg) was obtained as a colorless oily substance (yield 75%, syn/anti mixture)

출처 및 근거

ORD 기록
ord-229e7c4452d643f5bf3d904a69ab9b34
출처 데이터셋
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08183235B2

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