反応 #217002

反応方程式

1,3-Diaminoacetone dihydrochloride monohydrate

O-phenylmethylhydroxylamine hydrochloride

methanol

→

white material

収率 60.0%

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

収率 60.0%

反応条件

後処理

1. 1
   workup.ADDITIONwas added
2. 2
   温度After refluxing for 20 hours the solvent
3. 3
   その他was 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
   温度was heated to reflux
7. 7
   その他After 48 hours the solvent was removed in vacuo
8. 8
   その他Crystallization from methanol/ethyl acetate

実験手順

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.

出典