Ethanol → Ethyl 4-amino-3-methylbenzoate

HRID 1498897ノート

反応式

HRID 1498897 の反応式
[NH2:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][C:3]=1[CH3:11].[CH2:12](O)[CH3:13]>S(=O)(=O)(O)O>[NH2:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([O:8][CH2:12][CH3:13])=[O:7])=[CH:4][C:3]=1[CH3:11]

参加物

4

反応物 2

HCID 702EthanolHCID 755984-Amino-3-methylbenzoic acid

生成物 1

HCID 282796Ethyl 4-amino-3-methylbenzoate収率 99%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

To a suspension of 4-amino-3-methylbenzoic acid (5.00 g, 33.1 mmol) in ethanol (50 ml), concentrated sulfuric acid (5.00 ml) was slowly added. The mixture was heated under reflux for 3 hours. The solvent was distilled off under a reduced pressure. After the volume of the mixture was approximately halved, the mixture was neutralized with a saturated sodium bicarbonate solution. The mixture was subjected to extraction with ethyl acetate, and the extract was dried over anhydrous magnesium sulfate and then concentrated to give the title compound (5.87 g, 99%) as a light-brown solid.

後処理

  1. additionwas slowly added
  2. temperatureThe mixture was heated
  3. temperatureunder reflux for 3 hours
  4. distillationThe solvent was distilled off under a reduced pressure
  5. extractionThe mixture was subjected to extraction with ethyl acetate
  6. dry with materialthe extract was dried over anhydrous magnesium sulfate
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-d61fe132b4f64063afa55e42e5285956
出典データセット
uspto-grants-2015_12
特許番号
US09200008B2

反応ノート

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