Acetic Acid → 3',4'-Dihydroxyacetophenone

HRID 1395101

반응식

HRID 1395101 반응식
C(O)(=O)C.Cl[CH2:6][C:7]([C:9]1[CH:10]=[C:11]([OH:16])[C:12](=[CH:14][CH:15]=1)[OH:13])=[O:8]>O.C(O)C.[Zn]>[C:7]([C:9]1[CH:10]=[C:11]([OH:16])[C:12](=[CH:14][CH:15]=1)[OH:13])(=[O:8])[CH3:6]

참가 물질

6

반응물 2

HCID 176Acetic AcidHCID 668342-Chloro-3',4'-dihydroxyacetophenone

생성물 1

HCID 145303',4'-Dihydroxyacetophenone

시약·촉매·용매 3

HCID 23994Zinc촉매HCID 702Ethanol용매HCID 962Water용매

실험 절차

400 ml of a mixture of 1:8 v/v glacial acetic acid in water was added in two portions to a stirred mixture of 35 g of 4-(chloroacetyl)catechol in 300 ml of ethanol. At 10-minute intervals, four 10 g portions of 90% zinc dust were added, the mixture being held below about 45° C. The mixture then was stirred for 2 hours at 30°-40° C. and allowed to stand over a weekend. The liquid phase was decanted and stripped to a quarter of its volume under reduced pressure. The residue was extracted with ether. The ether extract was washed with sodium bicarbonate solution. The solvent was evaporated. The solid residue was recrystallized from toluene to give 4-acetylcatechol (1A), mp: 118°-119° C.

후처리

  1. custombeing held below about 45° C
  2. waitto stand over a weekend
  3. customThe liquid phase was decanted
  4. extractionThe residue was extracted with ether
  5. extractionThe ether extract
  6. washwas washed with sodium bicarbonate solution
  7. customThe solvent was evaporated
  8. customThe solid residue was recrystallized from toluene

출처 및 근거

ORD 기록
ord-3cdf5e18b8a5459786f5e3dee2f6db73
출처 데이터셋
uspto-grants-1980_05
특허 번호
US04202818

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