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

HRID 443598

반응식

HRID 443598 반응식
[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]

참가 물질

4

반응물 3

HCID 176Acetic AcidHCID 24813Phosphorus oxychlorideHCID 546829304-Hydroxycoumarin

생성물 1

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

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6e22ab87910c496b943fd3dbf46dcd95
출처 데이터셋
uspto-grants-1981_04
특허 번호
US04260776

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