Reacción #217002

Ecuación de reacción

1,3-Diaminoacetone dihydrochloride monohydrate

O-phenylmethylhydroxylamine hydrochloride

methanol

→

white material

Rendimiento 60.0%

1,6-Dihydro-5(4H)-pyrimidinone O-(phenylmethyl)oxime monohydrochloride

Rendimiento 60.0%

Condiciones de reacción

Tratamiento posterior

1. 1
   workup.ADDITIONwas added
2. 2
   TemperaturaAfter refluxing for 20 hours the solvent
3. 3
   Otrowas evaporated
4. 4
   workup.DISSOLUTIONThe crude product was dissolved in methanol
5. 5
   workup.ADDITIONan excess of trimethylorthoformate was added to the reaction mixture which
6. 6
   Temperaturawas heated to reflux
7. 7
   OtroAfter 48 hours the solvent was removed in vacuo
8. 8
   OtroCrystallization from methanol/ethyl acetate

Procedimiento

1,3-Diaminoacetone dihydrochloride monohydrate (2.00 g, 11.2 mmol) was dissolved in refluxing methanol and O-phenylmethylhydroxylamine hydrochloride (3.30 g, 20.5 mmol) was added. After refluxing for 20 hours the solvent was evaporated. The crude product was dissolved in methanol and an excess of trimethylorthoformate was added to the reaction mixture which was heated to reflux. After 48 hours the solvent was removed in vacuo. Crystallization from methanol/ethyl acetate afforded 1.60 g (60%) of white material. Mp. 167.5° C.

Fuente