تفاعل #1509585

معادلة التفاعل

(E)-3-amino-but-2-enenitrile

propynoic acid methyl ester

Dowtherm

→

2-Methyl-6-oxo-1,6-dihydro-pyridine-3-carbonitrile

المذيبات

DMF

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةrefluxed for additional 1 h
2. 2
   أخرىwas rised to 230° C
3. 3
   workup.DISTILLATIONDMF and MeOH were distilled off
4. 4
   درجة الحرارةThe reaction mixture was cooled down
5. 5
   workup.ADDITIONEtOAc (200 ml) was added
6. 6
   ترشيحthe resulting crystals were filtered off
7. 7
   غسيلwashed with EtOAc and ether affording the title compound (44.8 g, FP>250° C.)

الإجراء التجريبي

A solution of (E)-3-amino-but-2-enenitrile (100 g) and propynoic acid methyl ester in DMF (200 ml) was stirred at 25° C. for 2 h and refluxed for additional 1 h. Dowtherm (100 ml) was added and the temperature was rised to 230° C. DMF and MeOH were distilled off. The reaction mixture was cooled down, EtOAc (200 ml) was added and the resulting crystals were filtered off and washed with EtOAc and ether affording the title compound (44.8 g, FP>250° C.).

المصدر