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

HRID 577985ノート

反応式

HRID 577985 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-dc05634c906247dc8ab09044c6c4c294
出典データセット
uspto-grants-2015_05
特許番号
US09040528B2

反応ノート

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