تفاعل #217002

معادلة التفاعل

1,3-Diaminoacetone dihydrochloride monohydrate

O-phenylmethylhydroxylamine hydrochloride

methanol

→

white material

المردود 60.0%

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

المردود 60.0%

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONwas added
2. 2
   درجة الحرارةAfter refluxing for 20 hours the solvent
3. 3
   أخرىwas 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
   درجة الحرارةwas heated to reflux
7. 7
   أخرىAfter 48 hours the solvent was removed in vacuo
8. 8
   أخرىCrystallization from methanol/ethyl acetate

الإجراء التجريبي

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.

المصدر