반응 #684964

ord-78c996df416f467f9625a954b68b0ce5

반응 방정식

O=P(Cl)(Cl)Cl
Phosphorus oxychloride
CCCCc1ccc(CC(=O)NCC(O)c2cccc(OC)c2)cc1
compound
CCCCc1ccc(CC(=O)NCC(O)c2cccc(OC)c2)cc1
N-[2-Hydroxy-2-(3-methoxyphenyl)ethyl]-2-(4-butylphenyl)-acetamide
O=C([O-])O.[Na+]
sodium hydrogencarbonate
CCCCc1ccc(Cc2nccc3cc(OC)ccc23)cc1
title compound
수율 15.8%
CCCCc1ccc(Cc2nccc3cc(OC)ccc23)cc1
1-(4-Butylbenzyl)-6-methoxyisoquinoline
수율 15.8%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도under reflux for 1 hour 30 minutes
  2. 2
    온도The mixture was cooled on ice
  3. 3
    추출extracted with ethyl acetate
  4. 4
    건조dried over anhydrous magnesium sulfate
  5. 5
    농축concentrated under reduced pressure
  6. 6
    기타The residue was purified by silica gel column chromatography

실험 절차

Phosphorus oxychloride (1.6 ml) was added to a solution of the compound of Example B145 (600 mg, 1.7 mmol) in acetonitrile (15 ml), and the mixture was stirred under reflux for 1 hour 30 minutes. The mixture was cooled on ice, made alkaline with a 5% aqueous sodium hydrogencarbonate solution, extracted with ethyl acetate, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography to give the title compound (82 mg).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07897387B2uspto-grants-2011_03