反应详情

温度

4 °C

A solution of 5.47 g. (0.026 mole) of O-ethyl S-n-propyl phosphorochloridothioate in 20 ml. of acetonitrile is charged in one portion to a solution of 6.65 g. (0.025 mole) of 4-(benzenesulfonyloxy)thiophenol in 200 ml. of acetonitrile. The solution is stirred and cooled to 4° C. while 2.53 g. (0.025 mole) of triethylamine in 20 ml. of acetonitrile is added dropwise over a 30 minute period. The mixture is held at 5° C. for an additional hour and then concentrated in vacuo. The residue, a mixture of oil and solid, is taken up in 200 ml. of benzene and filtered to remove amine hydrochloride. The filtrate is washed once with 50 ml. of 5% sodium bicarbonate, once with 30 ml. of water, once with 30 ml. of saturated sodium chloride, dried over sodium sulfate, and concentrated in vacuo to give 9.1 g. (84%) of the phosphorodithioate as a pale yellow oil. Anal. calc. (found): C 47.2 (47.3); H 4.8 (5.15).

1. waitThe mixture is held at 5° C. for an additional hour
2. concentrationconcentrated in vacuo
3. additionThe residue, a mixture of oil and solid
4. filtrationof benzene and filtered
5. customto remove amine hydrochloride
6. washThe filtrate is washed once with 50 ml
7. dry with materialof saturated sodium chloride, dried over sodium sulfate
8. concentrationconcentrated in vacuo
9. customto give 9.1 g