تفاعل #684964

ord-78c996df416f467f9625a954b68b0ce5

معادلة التفاعل

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

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةunder reflux for 1 hour 30 minutes
  2. 2
    درجة الحرارةThe mixture was cooled on ice
  3. 3
    استخلاصextracted with ethyl acetate
  4. 4
    تجفيفdried over anhydrous magnesium sulfate
  5. 5
    تركيزconcentrated under reduced pressure
  6. 6
    أخرىThe residue was purified by silica gel column chromatography

الإجراء التجريبي

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).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07897387B2uspto-grants-2011_03