反应详情

Ethyl 3-(3-(trifluoromethyl)diaziridin-3-yl)benzoate (Preparation 199, 226 mg, 0.87 mmol) was stirred in methanol (10 mL) with triethylamine (0.36 mL, 2.61 mmol). Iodine (662 mg, 2.61 mmol) was dissolved in 2 mL methanol and added portion-wise until an orange-brown colour persisted. The reaction mixture was evaporated in vacuo and the residue was diluted with 1M aq. NaOH (30 mL) and then extracted with EtOAc (3×30 mL). The combined organic extracts were dried (MgSO4) and evaporated in vacuo to afford the title compound as a gum in 27% yield, 60 mg. This material was used in the next step without further purification.

1. additionadded portion-wise until an orange-brown colour
2. customThe reaction mixture was evaporated in vacuo
3. additionthe residue was diluted with 1M aq. NaOH (30 mL)
4. extractionextracted with EtOAc (3×30 mL)
5. dry with materialThe combined organic extracts were dried (MgSO4)
6. customevaporated in vacuo