HRID1873477
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
(4{[(trimethylsilyl)methyl]carbamoyl}naphthalen-1-yl)methyl acetate (2.0 g) and Lawesson reagent (2.4 g) were suspended with toluene (30 ml). The mixture was heated to reflux for 2 hours. The reaction mixture was returned to room temperature, washed with water and a saturated aqueous brine, subsequently dried over magnesium sulfate. After filtering the reaction mixture, the solvent was distilled off under reduced pressure, and the resulting mixture was purified by silica gel chromatography, to obtain (4{[(trimethylsilyl)methyl]carbamothioyl}naphthalen-1-yl)methyl acetate (1.2 g).
WORKUP
后处理
- temperatureThe mixture was heated
- temperatureto reflux for 2 hours
- customwas returned to room temperature
- washwashed with water
- dry with materiala saturated aqueous brine, subsequently dried over magnesium sulfate
- filtrationAfter filtering the reaction mixture
- distillationthe solvent was distilled off under reduced pressure
- customthe resulting mixture was purified by silica gel chromatography