تفاعل #1162466

معادلة التفاعل

3-oximino-2,4-pentanedione

d,l-norvaline

→

5-acetyl-4-methyl-2-propylimidazole

المردود 43.5%

المذيبات

acetonitrile

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwas heated
2. 2
   درجة الحرارةto reflux under nitrogen
3. 3
   درجة الحرارةto cool
4. 4
   ترشيحsuction filtered
5. 5
   غسيلThe residue was washed with acetonitrile
6. 6
   تركيزthe combined filtrates concentrated in vacuo
7. 7
   workup.DISSOLUTIONAfter dissolving the resulting oil in ethyl acetate (100 ml)
8. 8
   غسيلit was washed with three 40 ml portions of 5% aqueous sodium hydroxide solution
9. 9
   تجفيفThe combined organic extracts were dried over anhydrous potassium carbonate
10. 10
    تركيزconcentrated in vacuo

الإجراء التجريبي

An acetonitrile (250 ml) mixture of 3-oximino-2,4-pentanedione (40 g, 0.31 moles) and d,l-norvaline (43.55 g, 0.372 moles) was heated to reflux under nitrogen. After 23.7 h the reaction mixture was allowed to cool, then suction filtered. The residue was washed with acetonitrile and the combined filtrates concentrated in vacuo. After dissolving the resulting oil in ethyl acetate (100 ml), it was washed with three 40 ml portions of 5% aqueous sodium hydroxide solution. The combined organic extracts were dried over anhydrous potassium carbonate and then concentrated in vacuo to give 0.1 moles (43.5% yield based on recovered d,l-norvaline) of 5-acetyl-4-methyl-2-propylimidazole.

المصدر