تفاعل #518211

معادلة التفاعل

2,6-dimethyl pyridine

2-cyanobenzaldehyde

→

2-[2-(6-Methyl-pyridin-2-yl)-vinyl]-benzonitrile

المذيبات

acetic anhydride

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةunder reflux for 16 hours
2. 2
   أخرىThe acetic anhydride is then evaporated in vacuo
3. 3
   أخرىthe residue purified on column chromatography (silica gel 400 g)
4. 4
   غسيلThe column is first eluted with toluene (400 ml)
5. 5
   workup.ADDITIONThe fractions containing the desired compound
6. 6
   أخرىevaporated in vacuo
7. 7
   أخرىThe solid residue is recrystallized from methylene chloride/diisopropyl ether and white crystals
8. 8
   أخرىare isolated

الإجراء التجريبي

A solution of 2,6-dimethyl pyridine (5.8 ml, and 50 mMol), and 2-cyanobenzaldehyde (6.81 g, and 52 mMol) in acetic anhydride (9.5 ml) is heated under reflux for 16 hours. The acetic anhydride is then evaporated in vacuo and the residue purified on column chromatography (silica gel 400 g). The column is first eluted with toluene (400 ml) and then with toluene/ethyl acetate 95:5. The fractions containing the desired compound are combined, evaporated in vacuo. The solid residue is recrystallized from methylene chloride/diisopropyl ether and white crystals are isolated. (melting point: 113-114°).

المصدر