Methanol → Methyl 3,4-difluoro-2-hydroxybenzoate

HRID 245525노트

반응식

HRID 245525 반응식
[F:1][C:2]1[C:3]([OH:12])=[C:4]([CH:8]=[CH:9][C:10]=1[F:11])[C:5]([OH:7])=[O:6].S(=O)(=O)(O)O.[CH3:18]O>O>[F:1][C:2]1[C:3]([OH:12])=[C:4]([CH:8]=[CH:9][C:10]=1[F:11])[C:5]([O:7][CH3:18])=[O:6]

참가 물질

5

반응물 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 27582863,4-Difluoro-2-hydroxybenzoic acid

생성물 1

HCID 46311128Methyl 3,4-difluoro-2-hydroxybenzoate

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A solution of 3,4-difluoro-2-hydroxybenzoic acid (6.45 g, 37.05 mmol) and sulfuric acid (6 ml, 113 mmol) in MeOH (25 ml) was heated at reflux overnight. The mixture was diluted with water and extracted with ether. The ether was washed with aqueous NaHCO3, water and brine. The combined aqueous layers were twice more extracted with ether, which was washed with NaHCO3, water, and brine. The combined ether extracts were dried (MgSO4) and concentrated to give 6.4 g of product as a white solid.

후처리

  1. temperatureat reflux overnight
  2. extractionextracted with ether
  3. washThe ether was washed with aqueous NaHCO3, water and brine
  4. extractionThe combined aqueous layers were twice more extracted with ether, which
  5. washwas washed with NaHCO3, water, and brine
  6. dry with materialThe combined ether extracts were dried (MgSO4)
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-f5c6c7fa9aa14ced8a7b636a22e0ea39
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08658641B2

반응 노트

불러오는 중…