Acetic Acid → 3-Acetyl-4-hydroxy-2H-chromen-2-one

HRID 443598

反応式

HRID 443598 の反応式
[OH:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[O:5][C:4](=[O:12])[CH:3]=1.P(Cl)(Cl)(Cl)=O.[C:18](O)(=[O:20])[CH3:19]>>[C:18]([C:3]1[C:4](=[O:12])[O:5][C:6]2[C:11]([C:2]=1[OH:1])=[CH:10][CH:9]=[CH:8][CH:7]=2)(=[O:20])[CH3:19]

参加物

4

反応物 3

HCID 176Acetic AcidHCID 24813Phosphorus oxychlorideHCID 546829304-Hydroxycoumarin

生成物 1

HCID 546774033-Acetyl-4-hydroxy-2H-chromen-2-one

実験手順

120 g of 4-hydroxycoumarin in 600 ml of glacial acetic acid are heated to the boil and 380 ml of phosphorus oxychloride are added dropwise in the course of 60 minutes at the boil. The reaction mixture is heated to the boil under reflux for a further 30 minutes and is cooled and discharged into 4 l of ice-water. The crystalline residue is filtered off, washed with water and dried in vacuo at 50° C. 127 g of 3-acetyl-4-hydroxycoumarin are obtained.

後処理

  1. additionare added dropwise in the course of 60 minutes at the boil
  2. temperatureThe reaction mixture is heated to the boil
  3. temperatureunder reflux for a further 30 minutes
  4. temperatureis cooled
  5. filtrationThe crystalline residue is filtered off
  6. washwashed with water
  7. customdried in vacuo at 50° C

出典と根拠

ORDレコード
ord-6e22ab87910c496b943fd3dbf46dcd95
出典データセット
uspto-grants-1981_04
特許番号
US04260776

関連ノート

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