Methanol → Methyl 3-bromo-4-fluorobenzoate

HRID 851637

反応式

HRID 851637 の反応式
[F:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][C:3]=1[Br:11].S(=O)(=O)(O)O.[CH3:17]O>>[CH3:17][O:7][C:6](=[O:8])[C:5]1[CH:9]=[CH:10][C:2]([F:1])=[C:3]([Br:11])[CH:4]=1

参加物

4

反応物 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 705093-Bromo-4-fluorobenzoic acid

生成物 1

HCID 7018022Methyl 3-bromo-4-fluorobenzoate収率 97%

実験手順

A mixture of 87.6 g (0.38 mole) of 95% pure 4-fluoro-3-bromo-benzoic acid, 200 ml of methanol and 3 ml of sulphuric acid was boiled under for 18 hours. The excess methanol was then distilled off in vacuo, 300 ml of toluene were added and the solution was shaken first with 50 ml of water, then with 50 ml of saturated sodium bicarbonate solution and subsequently with 50 ml of water again. Thereafter, the solvent was distilled off in vacuo and the residue was distilled in vacuo. 86 g (97% of theory) of 4-fluoro-3-bromo-benzoic acid methyl ester were obtained in this manner in the form of a colorless oil which solidified as crystals when cold and had a boiling point of 64° C./0.1 mm Hg.

後処理

  1. customwas boiled under for 18 hours
  2. distillationThe excess methanol was then distilled off in vacuo, 300 ml of toluene
  3. additionwere added
  4. distillationThereafter, the solvent was distilled off in vacuo
  5. distillationthe residue was distilled in vacuo

出典と根拠

ORDレコード
ord-37b66a2622454b089a3cbaf65576ea6b
出典データセット
uspto-grants-1983_05
特許番号
US04386035

関連ノート

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