反应详情

温度

0 °C

2-Anthrol (3.0 grams; 0.015 mole), triethylamine (2.1 ml) and toluene (50 ml) were charged into a glass reaction vessel equipped with a mechanical stirrer and thermometer. The mixture was cooled to about 0° C. and O-ethyl S-propyl phosphorochloridothioate (3.01 grams; 0.015 mole) dissolved in toluene (38 ml) was added with stirring over a period of about 1/2 hour. After the addition was completed stirring was continued at room temperature overnight. After this time the reaction mixture was filtered to remove triethylamine hydrochloride and the filtrate stripped of solvent leaving solid residue. This residue was subjected to flash chromatography using ethyl acetate as the eluant to yield the desired product O-ethyl O-(2-anthryl) S-propyl phosphorothioate as a light tan solid melting at 79° to 83° C.

1. customequipped with a mechanical stirrer
2. additionwas added
3. additionAfter the addition
4. stirringwas completed stirring
5. waitwas continued at room temperature overnight
6. filtrationAfter this time the reaction mixture was filtered
7. customto remove triethylamine hydrochloride
8. customleaving solid residue