Acetic Acid → Butylcatechol

HRID 1029699

反応式

HRID 1029699 の反応式
[CH2:1]([C:5]1[CH:6]=[C:7]([O:13]C)[C:8](OC)=[CH:9][CH:10]=1)[CH2:2][CH2:3][CH3:4].Br.C(O)(=[O:18])C>>[CH2:1]([C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([OH:13])[C:6]=1[OH:18])[CH2:2][CH2:3][CH3:4]

参加物

4

反応物 3

HCID 176Acetic AcidHCID 260Hydrogen BromideHCID 5921764-Butyl-1,2-dimethoxybenzene

生成物 1

HCID 10192593Butylcatechol収率 80.6%

実験手順

A mixture of 5.64 g (29 mM) of 4-n-butylveratrole, 18.54 g (309 mM) of acetic acid and 55.62 g (323 mM) of 47% hydrobromic acid was heated under reflux for 4 hours with stirring. The reaction mixture was cooled to the room temperature and added with 50 ml of eater. The separated oil was extracted with ether. The ether solution was successively washed with 50 ml of water, 75 g of 5% aqueous sodium thiosulfate solution, and further twice with each 50 ml of water. The resulting solution was dried with anhydrous sodium sulfate, distilled off ether, and vacuum distilled to obtain 3.89 g (23 mM) of n-butylcatechol as light yellow liquid having a boiling point of 125° C./3 mmHg.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 4 hours
  3. additionadded with 50 ml of eater
  4. extractionThe separated oil was extracted with ether
  5. washThe ether solution was successively washed with 50 ml of water, 75 g of 5% aqueous sodium thiosulfate solution
  6. dry with materialThe resulting solution was dried with anhydrous sodium sulfate
  7. distillationdistilled off ether, and vacuum
  8. distillationdistilled

出典と根拠

ORDレコード
ord-62b652f4c501451db4df5795b1739ecf
出典データセット
uspto-grants-1992_04
特許番号
US05102906

関連ノート

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