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Methyl 4-oxo-4-(4-phenoxyphenyl)but-2-enoate → HCID 13276507, 화합물

HRID 2418151
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HRID 2418151 반응식
[O:1]([C:8]1[CH:21]=[CH:20][C:11]([C:12]([CH:14]=[CH:15][C:16]([O:18][CH3:19])=[O:17])=[O:13])=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:22]([OH:25])(=[S:24])[CH3:23]>C(OCC)C>[C:22]([S:24][CH:15]([CH2:14][C:12](=[O:13])[C:11]1[CH:20]=[CH:21][C:8]([O:1][C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)=[CH:9][CH:10]=1)[C:16]([O:18][CH3:19])=[O:17])(=[O:25])[CH3:23]
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참가 물질

4

반응물 2

HCID 53908224Methyl 4-oxo-4-(4-phenoxyphenyl)but-2-enoateHCID 178418634HCID 178418634, 화합물

생성물 1

HCID 13276507HCID 13276507, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

2.82 g of methyl 3-(4-phenoxybenzoyl)acrylate were dissolved in 30 ml of diethyl ether, then 1.5 ml of thioacetic acid were added. The mixture was stirred for 3 hours. The reaction mixture was washed, in turn, with water, a saturated aqueous solution of sodium hydrogencarbonate and water and then dried over magnesium sulfate. The diethyl ether was removed by distillation under reduced pressure. The residue was purified first by silica gel column chromatography, eluted with a mixture of hexane and diethyl ether, then by recrystallization from a mixture of hexane and diethyl ether to give 2.91 g of methyl 2-acetylthio-3-(4-phenoxybenzoyl)-propionate.

후처리

  1. washThe reaction mixture was washed, in turn, with water
  2. dry with materiala saturated aqueous solution of sodium hydrogencarbonate and water and then dried over magnesium sulfate
  3. customThe diethyl ether was removed by distillation under reduced pressure
  4. customThe residue was purified first by silica gel column chromatography
  5. washeluted with a mixture of hexane and diethyl ether
  6. customby recrystallization
  7. additionfrom a mixture of hexane and diethyl ether

출처 및 근거

ORD 기록
ord-5b703ee12b9a4357846b23280ce89c7a
출처 데이터셋
uspto-grants-1984_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04472316

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