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HCID 241612, 화합물 → HCID 13476441, 화합물

HRID 1981870
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HRID 1981870 반응식
[C:1]([CH:9]=[CH:10][C:11]([O:13][CH3:14])=[O:12])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:15]([OH:18])(=[S:17])[CH3:16]>C(OCC)C>[C:15]([S:17][CH:10]([CH2:9][C:1](=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)[C:11]([O:13][CH3:14])=[O:12])(=[O:18])[CH3:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 241612HCID 241612, 화합물HCID 178418634HCID 178418634, 화합물

생성물 1

HCID 13476441HCID 13476441, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

1.90 g of methyl 3-benzoylacrylate was dissolved in 30 ml of diethyl ether, and 0.8 ml of thioacetic acid was added thereto. The mixture was stirred for 5 hours at room temperature. The reaction solution was washed, in turn, with water, a saturated aqueous solution of sodium hydrogencarbonate and water, and dried over magnesium sulfate. The diethyl ether was removed from the solution by evaporation, and the residue was purified by silica gel column chromatography using a mixture of hexane and diethyl ether as an eluent, and then recrystallized from the same mixture to give 2.42 g of methyl 2-acetylthio-3-benzoylpropionate.

후처리

  1. washThe reaction solution was washed, in turn, with water
  2. dry with materiala saturated aqueous solution of sodium hydrogencarbonate and water, and dried over magnesium sulfate
  3. customThe diethyl ether was removed from the solution by evaporation
  4. customthe residue was purified by silica gel column chromatography
  5. additiona mixture of hexane and diethyl ether as an eluent
  6. customrecrystallized from the same mixture

출처 및 근거

ORD 기록
ord-08391010ad0b45479b52f0b2621adecc
출처 데이터셋
uspto-grants-1986_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04594197

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