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Acetic Acid → 4-Hydroxy-3-phenylbenzoic acid

HRID 326395
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HRID 326395 반응식
[C:1]1([C:7]2[CH:8]=[C:9]([CH:13]=[CH:14][C:15]=2[O:16]CC)[C:10]([OH:12])=[O:11])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(O)(=O)C>O>[C:1]1([C:7]2[CH:8]=[C:9]([CH:13]=[CH:14][C:15]=2[OH:16])[C:10]([OH:12])=[O:11])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 176Acetic AcidHCID 19736806HCID 19736806, 화합물

생성물 1

HCID 115865494-Hydroxy-3-phenylbenzoic acid

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A solution of 3-phenyl-4-ethoxybenzoic acid (26.6 g, 0.110 mole) and 550 ml of acetic acid was added to a one-liter, three-necked, round-bottom flask equipped with a 250 ml pressure equalizing dropping funnel, thermometer, cold water condenser, nitrogen inlet adapter and a polytetrafluoroethylene-coated magnetic stir bar. The flask was purged with nitrogen and the solution was brought to reflux. Approximately 125 ml of a 48 weight percent solution of HBr was added dropwise over fifteen minutes to the refluxing solution. The solution was refluxed for 30 hours. Without cooling, the solvent was rotary evaporated off leaving a slurry of a pinkish solid. The slurry was poured into one liter of deionized water and the mixture was stirred for one hour and filtered. The filter cake was dried in an 80° C. vacuum oven for three hours yielding 3-phenyl-4-hydroxybenzoic acid.

후처리

  1. customthree-necked, round-bottom flask equipped with a 250 ml pressure
  2. customThe flask was purged with nitrogen
  3. temperatureto reflux
  4. additionApproximately 125 ml of a 48 weight percent solution of HBr was added dropwise over fifteen minutes to the refluxing solution
  5. temperatureThe solution was refluxed for 30 hours
  6. temperatureWithout cooling
  7. customthe solvent was rotary evaporated off
  8. customleaving a slurry of a pinkish solid
  9. filtrationfiltered
  10. customThe filter cake was dried in an 80° C. vacuum oven for three hours

출처 및 근거

ORD 기록
ord-b8a7b72ce46746f1aa79954bf53f4ea6
출처 데이터셋
uspto-grants-1993_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05268443

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