تفاعل #65769

معادلة التفاعل

3-amino-6-bromo-4,5-diethoxycarbonyl-2-phenylpyridine

hydrazine monohydrate

→

8-Amino-5-bromo-7-phenylpyrido[3,4-d]pyridazine-1,4(2H,3H)dione

المذيبات

ethanol

ظروف التفاعل

المعالجة

1. 1
   workup.DISTILLATIONAfter the solvent was distilled off
2. 2
   ترشيحthe resulting crystals were collected by filtration with ethanol
3. 3
   workup.ADDITIONWater was added to the crystals
4. 4
   ترشيحthe resulting crystals were collected by filtration
5. 5
   workup.DISSOLUTIONThe crystals were dissolved in a small volume of methanol
6. 6
   workup.ADDITIONAfter mixing the methanol solution
7. 7
   أخرىwith silica gel, purification by silica gel column chromatography (eluent:ethyl acetate→ethylacetate/methanol 1:1)
8. 8
   ترشيحfollowed by collection by filtration

الإجراء التجريبي

In a mixture of 1 ml of ethanol and 2 ml of hydrazine monohydrate was dissolved 90 mg of 3-amino-6-bromo-4,5-diethoxycarbonyl-2-phenylpyridine, and the mixture was stirred for 2 hours at room temperature. After the solvent was distilled off, the resulting crystals were collected by filtration with ethanol. Water was added to the crystals, and the mixture was neutralized with 1N hydrochloric acid, the resulting crystals were collected by filtration. The crystals were dissolved in a small volume of methanol. After mixing the methanol solution with silica gel, purification by silica gel column chromatography (eluent:ethyl acetate→ethylacetate/methanol 1:1) was conducted, followed by collection by filtration.

المصدر