تفاعل #464744

معادلة التفاعل

Hydrazine hydrate

N-(3,5-dichlorophenyl)-2-(2,3-dihydro-6-formyl-4-oxo-5-phenyl-4H-1,3-oxazine-3-yl)-2-methylpropanamide

ethanol

→

N-(3,5-dichlorophenyl)-2-(6-aminoiminomethylene-2,3-dihydro-4-oxo-5-phenyl-4H-1,3-oxazin-3-yl)-2-methylpropanamide

ظروف التفاعل

المعالجة

1. 1
   أخرىAfter 0.5 hours the solvent was evaporated
2. 2
   workup.DISSOLUTIONthe residue dissolved in ethyl acetate
3. 3
   غسيلwashed with water and brine
4. 4
   تجفيفdried (magnesium sulphate)
5. 5
   أخرىevaporated
6. 6
   أخرىThe residue was purified
7. 7
   أخرىby dry column chromatography on silica gel
8. 8
   غسيلeluting with hexane/ethyl acetate

الإجراء التجريبي

Hydrazine hydrate (0.06 ml) was added to a stirred solution of N-(3,5-dichlorophenyl)-2-(2,3-dihydro-6-formyl-4-oxo-5-phenyl-4H-1,3-oxazine-3-yl)-2-methylpropanamide (0.5 g) in ethanol at room temperature. After 0.5 hours the solvent was evaporated, the residue dissolved in ethyl acetate and washed with water and brine, dried (magnesium sulphate) and evaporated. The residue was purified by dry column chromatography on silica gel, eluting with hexane/ethyl acetate to give N-(3,5-dichlorophenyl)-2-(6-aminoiminomethylene-2,3-dihydro-4-oxo-5-phenyl-4H-1,3-oxazin-3-yl)-2-methylpropanamide (compound 119, 0.19 g) as a pale yellow solid, m.p. 153-155° C.

المصدر