HRID1758307
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
1-Methyl-5-mercapto-1,2,3,4-tetrazole (1.2 g), potassium carbonate (2.1 g) and 3-chloropropyl 2-naphthyl ketone (3.5 g) are added to acetone (50 ml) and the mixture is refluxed with stirring for 2 hours. The reaction mixture is concentrated to dryness under reduced pressure and the residue dissolved in chloroform. Insolubles are filtered off. The filtrated is concentrated and the residue is purified by silica gel column chromatography [Kieselgel 60, eluant: benzene-ether (10:1)] and the product is recrystallized from ethanol to obtain 1-methyl-5-[3-(2-naphthoyl)propyl]thio-1,2,3,4-tetrazole (yield 51%) as colorless prisms, m.p. 118°-120° C.
WORKUP
后处理
- temperaturethe mixture is refluxed
- concentrationThe reaction mixture is concentrated to dryness under reduced pressure
- dissolutionthe residue dissolved in chloroform
- filtrationInsolubles are filtered off
- concentrationThe filtrated is concentrated
- customthe residue is purified by silica gel column chromatography [Kieselgel 60, eluant: benzene-ether (10:1)]
- customthe product is recrystallized from ethanol