Methanol → HCID 22955958, 화합물

HRID 508435노트

반응식

HRID 508435 반응식
[CH3:1][C:2]1[C:10]([F:11])=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[C:4]([F:12])[CH:3]=1.S(=O)(=O)(O)O.[CH3:18]O>>[F:12][C:4]1[CH:3]=[C:2]([CH3:1])[C:10]([F:11])=[CH:9][C:5]=1[C:6]([O:8][CH3:18])=[O:7]

참가 물질

4

반응물 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 136574512,5-Difluoro-4-methylbenzoic acid

생성물 1

HCID 22955958HCID 22955958, 화합물

실험 절차

To a suspension of 4-methyl-2,5-difluorobenzoic acid (comm, 52 g, 0.3 mol) in methanol (1.0 L) was added concentrated sulphuric acid (3 mL) with stirring and the reaction heated to reflux under nitrogen for 18 hours. The reaction was quenched with aqueous sodium bicarbonate solution (10%, 150 mL), concentrated in vacuo and the resulting residue partitioned between EtOAc (800 mL) and water (400 mL). The organic layer was washed with water (250 mL) and brine (100 mL), dried with sodium sulphate and concentrated in vacuo to yield the title compound as a clear oil that solidified on standing (54.7 g, 98%).

후처리

  1. temperaturethe reaction heated
  2. temperatureto reflux under nitrogen for 18 hours
  3. customThe reaction was quenched with aqueous sodium bicarbonate solution (10%, 150 mL)
  4. concentrationconcentrated in vacuo
  5. customthe resulting residue partitioned between EtOAc (800 mL) and water (400 mL)
  6. washThe organic layer was washed with water (250 mL) and brine (100 mL)
  7. dry with materialdried with sodium sulphate
  8. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-b91e4b8a228249349819a60b10c059e4
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09096500B2

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