反应详情

温度

100 °C

A mixture of NaH (60%, 31.8 mg, 0.79 mmol) and ethyl 2-(3-cyanopropyl)-1,3-dithiolane-2-carboxylate (171.5 mg, 0.66 mmol) in dioxane (5 mL) was heated at 100° C. overnight. The mixture was diluted with H2O and then extracted with ethyl acetate (×2). The combined organic layers were washed with brine, dried with Na2SO4, and evaporated to afford crude 6-oxo-1,4-dithiaspiro[4.4]nonane-7-carbonitrile: LCMS tR=1.67 Min (5 min run, UV254nm), Mass calculated for, M+213.0, observed LC/MS m/z 214.1 (M+H).

1. extractionextracted with ethyl acetate (×2)
2. washThe combined organic layers were washed with brine
3. dry with materialdried with Na2SO4
4. customevaporated