تفاعل #64959

معادلة التفاعل

water

sodium methylate

N-methylhydroxylamine hydrochloride

N-(2-methyl-prop-2-enyl)-N-(2-oxoethyl)-urethane

→

Ethyl 2,5-dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate

المذيبات

toluene

methanol

ظروف التفاعل

المعالجة

1. 1
   ترشيحThe sodium chloride is filtered off with suction
2. 2
   غسيلwashed with 8 ml of methanol and 80 ml of toluene
3. 3
   درجة الحرارةis heated
4. 4
   درجة الحرارةThe mixture is heated
5. 5
   درجة الحرارةunder reflux overnight
6. 6
   استخلاصthe product is extracted with 160 ml of 10% strength hydrochloric acid
7. 7
   استخلاصextracted with six portions, of 200 ml of CHCl3
8. 8
   تجفيفThe extracts are dried over K2CO3
9. 9
   تركيزconcentrated
10. 10
    workup.DISTILLATIONthe residue is distilled

الإجراء التجريبي

21.7 g of 30% strength sodium methylate solution are added dropwise to 10 g (0.12 mol) of N-methylhydroxylamine hydrochloride in 26 ml of methanol. The sodium chloride is filtered off with suction and washed with 8 ml of methanol and 80 ml of toluene. This solution is added dropwise to 19.2 g (0.11 mol) of N-(2-methyl-prop-2-enyl)-N-(2-oxoethyl)-urethane, which is heated under reflux in 160 ml of toluene using a water separator. The mixture is heated under reflux overnight, the product is extracted with 160 ml of 10% strength hydrochloric acid and the hydrochloric acid solution is rendered alkaline with potassium carbonate and extracted with six portions, of 200 ml of CHCl3. The extracts are dried over K2CO3 and concentrated and the residue is distilled.

المصدر