Ethanol → Ethyl 4-amino-3-methylbenzoate

HRID 1498897

반응식

HRID 1498897 반응식
[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]

참가 물질

4

반응물 2

HCID 702EthanolHCID 755984-Amino-3-methylbenzoic acid

생성물 1

HCID 282796Ethyl 4-amino-3-methylbenzoate수율 99%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d61fe132b4f64063afa55e42e5285956
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09200008B2

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