Ethanethiol → HCID 54717659, compound

Participants

Reaction Steps

4.45 ml (60 mmol) ethanethiol and 2.62 g (60 mmol, 60%) NaH were stirred for 15 mins. at room temperature in 100 ml DMF. 9.31 g (30 mmol) XIII were added to the resulting solution, followed by refluxing for 4 h. After hydrolysis with 25 ml saturated NH4Cl solution, the solvents were removed in vacuo, the residue was taken up in 500 ml ethyl acetate and washed with water. After drying over Na2SO4, flash chromatography (250 g SiO2, n-hexane:ethyl acetate=2:1+1% acetic acid), pre-adsorption: 25 g SiO2/CHCl3) yielded 6.89 g (23 mmol, 78%) XVI.

Provenance & Evidence