Methanol → Methyl 3-Amino-4-methoxybenzoate

HRID 349466

反応式

HRID 349466 の反応式
[NH2:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[O:11][CH3:12])[C:5]([OH:7])=[O:6].OS(O)(=O)=O.[CH3:18]O>>[CH3:18][O:6][C:5](=[O:7])[C:4]1[CH:8]=[CH:9][C:10]([O:11][CH3:12])=[C:2]([NH2:1])[CH:3]=1

参加物

4

反応物 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 178233-Amino-4-methoxybenzoic acid

生成物 1

HCID 2734814Methyl 3-Amino-4-methoxybenzoate収率 90%

実験手順

3-amino-4-methoxy benzoic acid (40 g, 0.239 mol) was dissolved in methanol, H2SO4 (38.14 ml, 0.717 mol) was added dropwise thereto and refluxed for 12 hours. The resulting mixture was cooled to room temperature and concentrated under a reduced pressure to remove methanol, neutralized with NaHCO3, extracted with ethyl acetate, and the extract was concentrated under a reduced pressure. The resulting residue was purified by recrystallization from ethyl acetate/hexane to obtain the title compound (39 g, 0.215 mol) in a yield of 90%.

後処理

  1. temperaturerefluxed for 12 hours
  2. concentrationconcentrated under a reduced pressure
  3. customto remove methanol
  4. extractionextracted with ethyl acetate
  5. concentrationthe extract was concentrated under a reduced pressure
  6. customThe resulting residue was purified by recrystallization from ethyl acetate/hexane

出典と根拠

ORDレコード
ord-56b670bf3a344ba1ad9a3b62c234d033
出典データセット
uspto-grants-2007_02
特許番号
US07179832B2

関連ノート

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