反应详情

A solution of N—BOC-1,1-dioxothiomorpholine (85 mg, 0.365 mmol) in a mixture of DCM (1 mL) and TFA (1 mL) was stirred at room temperature for 0.1 h before concentrating under vacuum and drying the TFA salt of 1,1-dioxothiomorpholine on the high vacuum pump for 3 h. The salt was dissolved in dry DMF (1 mL) and reacted with Example 22a (92 mg, 0.18 mmol) and K2CO3 (2.16 eq.) under General Procedure L. The crude mixture was purified by flash chromatography (silica gel, hexane/Et2O 1:4→MeOH/DCM 1:19) to afford 23 (14 mg, 14%) and 24 (13 mg, 13%) as clear colourless oils.

1. concentrationbefore concentrating under vacuum
2. dry with materialdrying the TFA salt of 1,1-dioxothiomorpholine on the high vacuum pump for 3 h
3. dissolutionThe salt was dissolved in dry DMF (1 mL)
4. customThe crude mixture was purified by flash chromatography (silica gel, hexane/Et2O 1:4→MeOH/DCM 1:19)