تفاعل #64975

معادلة التفاعل

sodium acetate

N-methylhydroxylamine hydrochloride

ethyl N-(but-2-enyl)-N-(2-oxoethyl)-carbamate

→

Ethyl 2,4-dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate

المذيبات

water

dioxane

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe mixture is heated
2. 2
   درجة الحرارةunder reflux overnight
3. 3
   درجة الحرارةcooled
4. 4
   ترشيحthe salts are filtered off with suction
5. 5
   غسيلwashed with dioxane
6. 6
   تركيزThe filtrate is concentrated
7. 7
   workup.ADDITIONK2CO3 is added
8. 8
   استخلاصThe mixture is extracted with CHCl3
9. 9
   تجفيفthe extract is dried over K2CO3
10. 10
    تركيزconcentrated
11. 11
    workup.DISTILLATIONthe residue is distilled

الإجراء التجريبي

18.4 g (0.1 mol) of ethyl N-(but-2-enyl)-N-(2-oxoethyl)-carbamate are dissolved in 100 ml of dioxane, and 9 g of anhydrous sodium acetate and 9 g (0.108 mol) of N-methylhydroxylamine hydrochloride in 10 ml of water are added. The mixture is heated under reflux overnight and cooled and the salts are filtered off with suction and washed with dioxane. The filtrate is concentrated, the residue is taken up in 100 ml of water and K2CO3 is added. The mixture is extracted with CHCl3, the extract is dried over K2CO3 and concentrated and the residue is distilled.

المصدر