反应详情

7.9 g (0.3 mol) of sodium in a stream of nitrogen was placed in a 500-ml 3-necked flash with reflux condenser, drying tube and dropping funnel with pressure equalisation. Next, 250 ml of anhydrous methanol was carefully added dropwise and agitated until the sodium had completely dissolved. A methanolic solution of 95.4 g (0.58 mol) malonic acid diethyl ester was added very slowly dropwise to the still-warm sodium methanolate solution. At the end of the addition process, the mixture was reflux-boiled for a further hour, after which 0.5 mol of 1-chloro-4-tetrahydro-pyranyloxybutane was slowly added dropwise. The mixture was then reflux-boiled overnight.

1. temperaturewith reflux condenser
2. customdrying tube
3. additionNext, 250 ml of anhydrous methanol was carefully added dropwise
4. dissolutionhad completely dissolved
5. waitAt the end of the addition process, the mixture was reflux-boiled for a further hour
6. customreflux-boiled overnight