反应详情

Dry hydrogen sulphide gas is passed for 10 minutes into a solution, cooled to 0° C., of 277 mg (1 mmol) of diethylphosphono-isocyanoacetic acid tert.-butyl ester in 5 ml of dry tetrahydrofurane (filtered through aluminium oxide). After adding a few crystals of copper-II acetylacetonate, the reaction vessel is closed and left to stand overnight at room temperature. The reaction mixture is filtered and the filtrate is evaporated in vacuo. The residue is chromatographed on silica gel thick layer plates with toluene/ethyl acetate, 1:1, and gives thioformamido-diethylphosphonoacetic acid tert.-butyl ester in the form of a colourless oil: IR spectrum (in methylene chloride): characteristic bands at 3.13; 3.35; 5.75; 7.01; 8.10; 8.70 and 9.75μ.

1. customthe reaction vessel is closed
2. waitleft
3. filtrationThe reaction mixture is filtered
4. customthe filtrate is evaporated in vacuo
5. customThe residue is chromatographed on silica gel thick layer plates with toluene/ethyl acetate, 1:1