Selenium Dioxide → 2-Methoxyphenylglyoxal hydrate

HRID 66318

반응식

HRID 66318 반응식
C[O:2][CH2:3][C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)=[O:5].[Se](=O)=O.[O:15]1CCOC[CH2:16]1>O.C(OCC)(=O)C>[OH2:2].[CH3:16][O:15][C:7]1[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=1[C:4]([CH:3]=[O:2])=[O:5]

참가 물질

6

반응물 3

HCID 24007Selenium DioxideHCID 312751,4-DioxaneHCID 776982-Methoxy-1-phenylethanone

생성물 1

HCID 204341102-Methoxyphenylglyoxal hydrate

시약·촉매·용매 2

HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

3 g of 2-methoxyacetophenone are dissolved in 15 ml of dioxane, and a solution of 3.3 g of selenium dioxide in 1.5 ml of water is added thereto. The solution is refluxed for 15 hours. After the reaction, insoluble materials are removed by filtration, and the filtrate is concentrated. The oily residue thus obtained is dissolved in ethyl acetate. The ethyl acetate solution is washed with water and then with an aqueous sodium bicarbonate solution and water. Then, said solution is dried and evaporated to remove solvent. 3.1 g of 2-methoxyphenylglyoxal hydrate are obtained as a crude oil.

후처리

  1. temperatureThe solution is refluxed for 15 hours
  2. customAfter the reaction, insoluble materials
  3. customare removed by filtration
  4. concentrationthe filtrate is concentrated
  5. customThe oily residue thus obtained
  6. washThe ethyl acetate solution is washed with water
  7. customis dried
  8. customevaporated
  9. customto remove solvent

출처 및 근거

ORD 기록
ord-d7ae0d83b4204e4da29186e8c627e9d9
출처 데이터셋
uspto-grants-1978_12
특허 번호
US04131686

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