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Methanol → HCID 18433366, 화합물

HRID 1372560
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HRID 1372560 반응식
[OH:1][C:2]1[CH:3]=[C:4]([CH2:11][C:12]([OH:14])=[O:13])[CH:5]=[CH:6][C:7]=1[N+:8]([O-:10])=[O:9].S(=O)(=O)(O)O.[CH3:20]O>>[OH:1][C:2]1[CH:3]=[C:4]([CH2:11][C:12]([O:14][CH3:20])=[O:13])[CH:5]=[CH:6][C:7]=1[N+:8]([O-:10])=[O:9]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 235083252-(3-Hydroxy-4-nitrophenyl)acetic acid

생성물 1

HCID 18433366HCID 18433366, 화합물

실험 절차

To 3-hydroxy-4-nitrophenylacetic acid (5.45 g, 27.6 mol) and methanol (100 ml) was added concentrated sulfuric acid (0.5 ml). The mixture was then heated under reflux for 4 hours under stirring. After cooling to room temperature, the reaction mixture was distilled under reduced pressure to remove the solvent. Water (100 ml) was added to the residue, followed by extraction with ether (300 ml). The extract was washed successively with a saturated aqueous solution (100 ml) of sodium bicarbonate and saturated brine (100 ml), dried over anhydrous magnesium sulfate and distilled under reduced pressure to remove the solvent, whereby the title compound (4.90 g, 84%) was obtained as a yellow crystalline powder.

후처리

  1. temperatureThe mixture was then heated
  2. temperatureunder reflux for 4 hours
  3. distillationthe reaction mixture was distilled under reduced pressure
  4. customto remove the solvent
  5. additionWater (100 ml) was added to the residue
  6. extractionfollowed by extraction with ether (300 ml)
  7. washThe extract was washed successively with a saturated aqueous solution (100 ml) of sodium bicarbonate and saturated brine (100 ml)
  8. dry with materialdried over anhydrous magnesium sulfate
  9. distillationdistilled under reduced pressure
  10. customto remove the solvent, whereby the title compound (4.90 g, 84%)
  11. customwas obtained as a yellow crystalline powder

출처 및 근거

ORD 기록
ord-c0881b3724bb42cbab29c72d617c7511
출처 데이터셋
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07157487B2

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