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
6-Trifluoromethyl-2-anthrol (0.01 mole), triethylamine (0.01 mole), tetrahydrofuran (25 ml) and toluene (25 ml) are charged into a glass reaction vessel equipped with a mechanical stirrer and thermometer. The mixture is cooled to a temperature of about 0° C. and O-(2,4-dimethylphenyl) S-propyl phosphorochloridothioate (0.01 mole) dissolved in toluene (25 ml) is added with stirring over a period of about 30 minutes. After the addition is completed the reaction mixture is allowed to warm to room temperature and stirring is continued for a period of about 16 hours. After this time the reaction mixture is filtered to remove triethylamine hydrochloride. The filtrate is then washed with water, dried over anhydrous magnesium sulfate and stripped of solvents leaving a residue. This residue is subjected to flash chromatography using ethyl acetate as the eluant to yield the desired product O-(2,4-dimethylphenyl) O-(6-trifluoromethyl-2-anthryl) S-propyl phosphorothioate.
WORKUP
后处理
- customequipped with a mechanical stirrer
- additionis added
- additionAfter the addition
- stirringstirring
- waitis continued for a period of about 16 hours
- filtrationAfter this time the reaction mixture is filtered
- customto remove triethylamine hydrochloride
- washThe filtrate is then washed with water
- dry with materialdried over anhydrous magnesium sulfate
- customleaving a residue