Hydrochloric Acid → 1-(6-Hydroxy-2-naphthyl)ethan-1-one

HRID 431433

反応式

HRID 431433 の反応式
Cl.C[O:3][C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][CH:13]=1)[CH:10]=[C:9]([C:14](=[O:16])[CH3:15])[CH:8]=[CH:7]2>ClCCl>[OH:3][C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][CH:13]=1)[CH:10]=[C:9]([C:14](=[O:16])[CH3:15])[CH:8]=[CH:7]2

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 775062-Acetyl-6-methoxynaphthalene

生成物 1

HCID 826311-(6-Hydroxy-2-naphthyl)ethan-1-one収率 89%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

In a 3 L two-neck round bottom flask, equipped with a reflux condenser and a dropping funnel, 2 L of hydrochloric acid (d=1.16) were stirred and heated to boiling. A solution of 6.06 g (30.3 mmol) of 1-(6-methoxy-2-naphthyl)-1-ethanone (prepared as described in Arsenijevic et al., Org. Synth. Coll. 6:34 (1988), the disclosure of which is incorporated herein by reference) in a minimum amount of dichloromethane was added, and the mixture was stirred and heated at reflux for 2 hours. The hot solution was filtered through a mineral wool plug to remove oily residue. The solid that separated after cooling was filtered on a glass frit and dissolved in 130 mL of ethyl acetate. The solution was washed with brine, dried with anhydrous magnesium sulfate and evaporated to give 5 g (89%) of 1-(6-hydroxy-2-naphthyl)1-ethanone.

後処理

  1. customIn a 3 L two-neck round bottom flask, equipped with a reflux condenser and a dropping funnel
  2. temperatureheated to boiling
  3. additionwas added
  4. temperatureheated
  5. temperatureat reflux for 2 hours
  6. filtrationThe hot solution was filtered through a mineral wool plug
  7. customto remove oily residue
  8. customThe solid that separated
  9. temperatureafter cooling
  10. filtrationwas filtered on a glass frit
  11. dissolutiondissolved in 130 mL of ethyl acetate
  12. washThe solution was washed with brine
  13. dry with materialdried with anhydrous magnesium sulfate
  14. customevaporated

出典と根拠

ORDレコード
ord-babaac4f6d4d4070ad7fa7e79755f2c3
出典データセット
uspto-grants-2003_12
特許番号
US06660530B2

関連ノート

読み込み中…