Methanol → Methyl 3-chloro-4-hydroxyphenylacetate

HRID 247971

反応式

HRID 247971 の反応式
[Cl: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]([Cl:1])[CH:3]=1

参加物

5

反応物 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 1185343-Chloro-4-hydroxyphenylacetic acid

生成物 1

HCID 92625Methyl 3-chloro-4-hydroxyphenylacetate

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 50 g of 3-chloro-4-hydroxybenzeneacetic acid, 250 ml of methyl alcohol and 10 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 saturated sodium bicarbonate and saturated sodium chloride, dried and concentrated in vacuo. The residue is purified by column chromatography (silica gel:30% ethyl acetate/hexane) to give 49.9 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 saturated sodium bicarbonate and saturated sodium chloride
  5. customdried
  6. concentrationconcentrated in vacuo
  7. customThe residue is purified by column chromatography (silica gel:30% ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-ac4d11a90ae84fd68317a962f0878cda
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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