반응 #4267

반응 방정식

diethyl methylmalonate

propargyl bromide

sodium bromide

→

Diethyl 2-methyl-2-propargyl-malonate

용매

반응 조건

후처리

1. 1
   기타At 35° to 40°
2. 2
   workup.STIRRINGthe mixture is stirred for a further hour
3. 3
   기타at 45° C
4. 4
   온도The mixture is refluxed for a further 2 hours
5. 5
   기타is separated by suction
6. 6
   여과filtering
7. 7
   기타the filtrate is substantially evaporated in vacuo
8. 8
   workup.STIRRINGThe residue is stirred into ice water
9. 9
   추출the aqueous solution is extracted several times with ether
10. 10
    기타The combined organic phases are dried
11. 11
    기타evaporated to dryness in vacuo
12. 12
    기타The resulting oil is used in the next stage without any further purification

실험 절차

At 35° to 40° to C., with stirring, 174 g (1.0 ml) of diethyl methylmalonate are added dropwise to an alkoxide solution (prepared from 23 g of sodium and 800 ml of absolute ethanol), the mixture is stirred for a further hour and then at 45° C. 130.8 g (1.1 mol) of propargyl bromide are added dropwise. The mixture is refluxed for a further 2 hours. After cooling the precipitated sodium bromide is separated by suction filtering and the filtrate is substantially evaporated in vacuo. The residue is stirred into ice water and the aqueous solution is extracted several times with ether. The combined organic phases are dried and evaporated to dryness in vacuo. The resulting oil is used in the next stage without any further purification.

출처