反应 #684964

ord-78c996df416f467f9625a954b68b0ce5

反应方程式

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
收率 15.8%
CCCCc1ccc(Cc2nccc3cc(OC)ccc23)cc1
1-(4-Butylbenzyl)-6-methoxyisoquinoline
收率 15.8%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度under reflux for 1 hour 30 minutes
  2. 2
    温度The mixture was cooled on ice
  3. 3
    萃取extracted with ethyl acetate
  4. 4
    干燥dried over anhydrous magnesium sulfate
  5. 5
    浓缩concentrated under reduced pressure
  6. 6
    其他The residue was purified by silica gel column chromatography

实验过程

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).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07897387B2uspto-grants-2011_03