HRID1249066
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 (3RS)-1,2,3,4-tetrahydro-β-carboline-3-carboxylate (2.30 g) is dissolved in methanol (50 ml) and thereto are added triethylamine (1.21 g) and carbon disulfide (920 mg). The mixture is stirred at room temperature for 20 minutes and thereto is added dropwise methyl iodide (1.70 g). The mixture is stirred for 4 hours and distilled under reduced pressure to remove the solvent. The residue is dissolved in ethyl acetate, and the mixture is washed with water, dried and distilled to remove the solvent. The residue is recrystallized from ether-n-hexane to give the title compound (2.10 g, 65.6%) as colorless needles, m.p. 132°-134° C.
WORKUP
后处理
- stirringThe mixture is stirred for 4 hours
- distillationdistilled under reduced pressure
- customto remove the solvent
- dissolutionThe residue is dissolved in ethyl acetate
- washthe mixture is washed with water
- customdried
- distillationdistilled
- customto remove the solvent
- customThe residue is recrystallized from ether-n-hexane