4'-Hydroxyacetophenone → 4-Hydroxyphenylglyoxal

HRID 653046

反応式

HRID 653046 の反応式
[CH3:1][C:2]([C:4]1[CH:5]=[CH:6][C:7]([OH:10])=[CH:8][CH:9]=1)=[O:3].[O:11]1CCOCC1>O>[OH:10][C:7]1[CH:8]=[CH:9][C:4]([C:2]([CH:1]=[O:11])=[O:3])=[CH:5][CH:6]=1

参加物

4

反応物 2

HCID 74694'-HydroxyacetophenoneHCID 312751,4-Dioxane

生成物 1

HCID 905684-Hydroxyphenylglyoxal

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

4-Hydroxyacetophenone (15 g., 0.11 mol) was dissolved in 70 ml. dioxane and 8.3 ml. H2O. SeO2 (12.2 g., 0.11 mol) was added and the mixture heated at 80° for 18 hours, then filtered over diatomaceous earth. The filtrate was stripped, taken up in 150 ml. H2O, heated on a steam bath, decolorized with activated carbon, cooled to refrigerator temperature, and hydrate of title product recovered by filtration, 5.72 g. Anhydrous title product was obtained by Kugelrohr distillation; 1H-nmr 5.97 (s, 1H), 6.97 (d, 2H, J=6 Hz), 8.22 (d, 2H, J=6 Hz), 9.68 (s, 1H).

後処理

  1. temperaturethe mixture heated at 80° for 18 hours
  2. filtrationfiltered over diatomaceous earth
  3. temperatureH2O, heated on a steam bath
  4. temperaturecooled to refrigerator temperature, and hydrate of title product
  5. filtrationrecovered by filtration, 5.72 g

出典と根拠

ORDレコード
ord-7635795a240444e6a859abac41a4658c
出典データセット
uspto-grants-1987_06
特許番号
US04675186

関連ノート

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