반응 #217002

반응 방정식

1,3-Diaminoacetone dihydrochloride monohydrate

O-phenylmethylhydroxylamine hydrochloride

methanol

→

white material

수율 60.0%

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

수율 60.0%

반응 조건

후처리

1. 1
   workup.ADDITIONwas added
2. 2
   온도After refluxing for 20 hours the solvent
3. 3
   기타was 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
   온도was heated to reflux
7. 7
   기타After 48 hours the solvent was removed in vacuo
8. 8
   기타Crystallization from methanol/ethyl acetate

실험 절차

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.

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