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

HRID 650447

반응식

HRID 650447 반응식
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

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 775062-Acetyl-6-methoxynaphthalene

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-da4f1c131c9e4829b205d595b615ca32
출처 데이터셋
uspto-grants-2001_08
특허 번호
US06274119B1

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