HRID1979985

反应详情

EQUATION

反应方程式

HRID 1979985 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. dissolutionto dissolve
  2. extractionthe mixture extracted four times with (4×) 500 ml of ether
  3. dry with materialThe combined ether extracts were dried over sodium sulfate
  4. customthe ether evaporated under reduced pressure
  5. customusing a 40°
  6. distillationThe methyl 1,2,5,6-tetrahydro-1-methylnicotinate was distilled under aspirator vacuum