Reaktion #217002

Reaktionsgleichung

1,3-Diaminoacetone dihydrochloride monohydrate

O-phenylmethylhydroxylamine hydrochloride

methanol

→

white material

Ausbeute 60.0%

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

Ausbeute 60.0%

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwas added
2. 2
   TemperaturAfter refluxing for 20 hours the solvent
3. 3
   Sonstigewas 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
   Temperaturwas heated to reflux
7. 7
   SonstigeAfter 48 hours the solvent was removed in vacuo
8. 8
   SonstigeCrystallization from methanol/ethyl acetate

Vorschrift

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.

Quelle