تفاعل #1509586
ord-7cdb17f067a04e22aa9305970d553803
معادلة التفاعل
2-Methyl-6-oxo-1,6-dihydro-pyridine-3-carbonitrile
POCl3
→
title compound
6-Chloro-2-methyl-nicotinonitrile
الكواشف
لا شيء
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1درجة الحرارةwas refluxed for 3 h
- 2أخرىThe reaction mixture was dried down in vacuum and ice
- 3workup.ADDITIONwas added
- 4استخلاصThe aqueous layer was extracted with EtOAc
- 5أخرىThe organic layer was separated
- 6أخرىdried
- 7تركيزconcentrated 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.).