Methanol → Methyl 2-(3-fluoro-4-hydroxyphenyl)acetate

HRID 247969

反応式

HRID 247969 の反応式
[F:1][C:2]1[CH:3]=[C:4]([CH2:9][C:10]([OH:12])=[O:11])[CH:5]=[CH:6][C:7]=1[OH:8].[CH3:13]O.S(=O)(=O)(O)O>O>[CH3:13][O:11][C:10](=[O:12])[CH2:9][C:4]1[CH:5]=[CH:6][C:7]([OH:8])=[C:2]([F:1])[CH:3]=1

参加物

5

反応物 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 680143-Fluoro-4-hydroxybenzeneacetic acid

生成物 1

HCID 10797559Methyl 2-(3-fluoro-4-hydroxyphenyl)acetate

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 2.0 g of 3-fluoro-4-hydroxybenzeneacetic acid, 10 ml of methyl alcohol and 1 ml of concentrated sulfuric acid is heated at reflux temperature for 23.5 hours. The cooled solution is diluted with water and extracted with methylene chloride. The organic layer is washed with water, saturated sodium bicarbonate, water and saturated sodium chloride; dried and concentrated in vacuo. The residue is purified by column chromatography (silica gel:25% ethyl acetate/hexane) to give 1.9 g of the desired product.

後処理

  1. temperatureis heated
  2. temperatureat reflux temperature for 23.5 hours
  3. extractionextracted with methylene chloride
  4. washThe organic layer is washed with water, saturated sodium bicarbonate, water and saturated sodium chloride
  5. customdried
  6. concentrationconcentrated in vacuo
  7. customThe residue is purified by column chromatography (silica gel:25% ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-1b4c5b4238094374b404e5e81d4d6beb
出典データセット
uspto-grants-1993_05
特許番号
US05208247

関連ノート

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