反应详情

Reflux a mixture of 1-dimethylcarbamoylthio-4-(1,1-dimethyl-propyl)-benzene (520 mg, 2.1 mmol) and K2CO3 (1.28 g, 9.3 mmol) in methanol (40 mL) for 6 h. Cool to room temperature and concentrate in vacuo. Suspend the residue in water and acidify to pH 1 with 1M aqueous HCl. Extract the aqueous phase with EtOAc (3×40 mL). Dry the combined organic extracts over MgSO4, filter and concentrate in vacuo. Purify the crude mixture by chromatography on silica gel eluting with hexane/EtOAc (1:0 to 97:3) to obtain the title compound (100 mg, 26%).

1. temperatureReflux
2. concentrationconcentrate in vacuo
3. extractionExtract the aqueous phase with EtOAc (3×40 mL)
4. dry with materialDry the combined organic extracts over MgSO4
5. filtrationfilter
6. concentrationconcentrate in vacuo
7. customPurify the crude mixture by chromatography on silica gel eluting with hexane/EtOAc (1:0 to 97:3)