تفاعل #1509586

ord-7cdb17f067a04e22aa9305970d553803

معادلة التفاعل

Cc1[nH]c(=O)ccc1C#N
2-Methyl-6-oxo-1,6-dihydro-pyridine-3-carbonitrile
O=P(Cl)(Cl)Cl
POCl3
Cc1nc(Cl)ccc1C#N
title compound
Cc1nc(Cl)ccc1C#N
6-Chloro-2-methyl-nicotinonitrile

الكواشف

لا شيء

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas refluxed for 3 h
  2. 2
    أخرىThe reaction mixture was dried down in vacuum and ice
  3. 3
    workup.ADDITIONwas added
  4. 4
    استخلاصThe aqueous layer was extracted with EtOAc
  5. 5
    أخرىThe organic layer was separated
  6. 6
    أخرىdried
  7. 7
    تركيزconcentrated in vacuum

الإجراء التجريبي

A mixture of 2-Methyl-6-oxo-1,6-dihydro-pyridine-3-carbonitrile (44 g) and POCl3 (250 ml) was refluxed for 3 h. The reaction mixture was dried down in vacuum and ice followed by conc. aqueous ammonia (300 ml) was added. The aqueous layer was extracted with EtOAc. The organic layer was separated, dried and concentrated in vacuum affording the title compound (23.5 g, BP (18 mbar) 119-120° C.).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: USRE045323E1uspto-grants-2015_01