Methanol → Methyl 2-Amino-5-methylbenzoate

HRID 653705ノート

反応式

HRID 653705 の反応式
[NH2:1][C:2]1[CH:10]=[CH:9][C:8]([CH3:11])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].S(=O)(=O)(O)O.[CH3:17]O>>[NH2:1][C:2]1[CH:10]=[CH:9][C:8]([CH3:11])=[CH:7][C:3]=1[C:4]([O:6][CH3:17])=[O:5]

参加物

4

反応物 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 762552-Amino-5-methylbenzoic acid

生成物 1

HCID 1201104Methyl 2-Amino-5-methylbenzoate収率 74%

実験手順

A mixture of 2-amino-5-methyl benzoic acid (10 g) in methanol (50 ml) containing conc. sulfuric acid (5.5 ml) was heated for 19 hours under reflux. The solvent was distilled off, and the residue was dissolved in water. The solution was neutralized with an aqueous sodium hydroxide, followed by extraction with ethyl acetate. The organic layer was dried and concentrated to afford a pale brown oil (8.1 g, 74%).

後処理

  1. temperaturewas heated for 19 hours
  2. temperatureunder reflux
  3. distillationThe solvent was distilled off
  4. dissolutionthe residue was dissolved in water
  5. extractionfollowed by extraction with ethyl acetate
  6. customThe organic layer was dried
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-bc92e83984b842d8837982b28305a6a3
出典データセット
uspto-grants-1992_07
特許番号
US05128356

反応ノート

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