تفاعل #77858

معادلة التفاعل

3-bromo-tetrahydropyran-2-ol

formamidine acetate

diethylamine

N,N-dimethylformamide

→

3-(1H-imidazol-4-yl)propanol oxalate

المردود 42.0%

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONwas added dropwise
2. 2
   workup.DISTILLATIONdistilled in vacuo for about 1 hour at the same temperature
3. 3
   أخرىto remove the solvent
4. 4
   workup.ADDITIONThe resulting oily residue was diluted with 25 ml of acetone and 4.97 g of oxalic acid
5. 5
   workup.ADDITIONwas slowly added
6. 6
   أخرىfor crystallization
7. 7
   workup.STIRRINGThe reaction mixture was stirred for about 1 hour
8. 8
   ترشيحfiltered
9. 9
   غسيلwashed with acetone

الإجراء التجريبي

5.0 g of 3-bromo-tetrahydropyran-2-ol prepared in Example 1 and 5.75 g of formamidine acetate were added to 25 ml of N,N-dimethylformamide and 9 ml of diethylamine was added dropwise thereto. The reaction mixture was stirred for about 4 hours at 80° C. and distilled in vacuo for about 1 hour at the same temperature to remove the solvent. The resulting oily residue was diluted with 25 ml of acetone and 4.97 g of oxalic acid was slowly added thereto for crystallization. The reaction mixture was stirred for about 1 hour, filtered, and washed with acetone to give 2.5 g of 3-(1H-imidazol-4-yl)propanol oxalate (yield: 42%).

المصدر