HRID1979985
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Methyl 1,2,5,6-tetrahydro-1-methylnicotinate hydrobromide (Arecoline HBr) weighing 350 g, was dissolved in 600 ml of water. To this solution 50 g of sodium chloride was added and allowed to dissolve. To this solution approximately 400 ml of saturated sodium carbonate solution was added and the mixture extracted four times with (4×) 500 ml of ether. The combined ether extracts were dried over sodium sulfate and the ether evaporated under reduced pressure using a 40° water bath. The methyl 1,2,5,6-tetrahydro-1-methylnicotinate was distilled under aspirator vacuum to give 188 g (82%) of a pale yellow liquid with b.p. 85°/20 mm (pressure approximate). The free base was stored in a freezer.
WORKUP
后处理
- dissolutionto dissolve
- extractionthe mixture extracted four times with (4×) 500 ml of ether
- dry with materialThe combined ether extracts were dried over sodium sulfate
- customthe ether evaporated under reduced pressure
- customusing a 40°
- distillationThe methyl 1,2,5,6-tetrahydro-1-methylnicotinate was distilled under aspirator vacuum