تفاعل #77859

معادلة التفاعل

3-bromo-2-methyl-tetrahydrofuran-2-ol

formamidine acetate

N,N-dimethylformamide

diethylamine

→

2-(5-methyl-1H-imidazol-4-yl)ethanol oxalate

المردود 42.0%

ظروف التفاعل

المعالجة

1. 1
   workup.DISTILLATIONwas distilled in vacuo for about 1 hour at the same temperature
2. 2
   workup.ADDITIONThe resulting oily residue was diluted with 25 ml of acetone
3. 3
   workup.ADDITION4.95 g of oxalic acid was added to the reaction mixture, which
4. 4
   workup.STIRRINGwas then stirred for about 1 hour
5. 5
   ترشيحThe resulting solid was filtered
6. 6
   غسيلwashed with acetone

الإجراء التجريبي

5.0 g of 3-bromo-2-methyl-tetrahydrofuran-2-ol and 5.75 g of formamidine acetate were added to 15 ml of N,N-dimethylformamide. 5 g of diethylamine was slowly added to the reaction mixture, which was then stirred for about 4 hours at 80° C. and was distilled in vacuo for about 1 hour at the same temperature. The resulting oily residue was diluted with 25 ml of acetone. 4.95 g of oxalic acid was added to the reaction mixture, which was then stirred for about 1 hour. The resulting solid was filtered and washed with acetone to give 2.5 g of 2-(5-methyl-1H-imidazol-4-yl)ethanol oxalate (yield: 42%).

المصدر