反应详情

To a solution of commercially available 4-chlorophenyl glyoxylohydroxamyl chloride (218 mg, 1 mmol) in 1,1,1-trifluoro-2-trifluoromethyl-but-3-en-2-ol (2 mmol) was added a solution of triethylamine (111 mg, 1.1 mmol) in THF (10 ml) dropwise by syringe pump at r.t. over 30 h. The mixture was concentrated under reduced pressure and diluted with EtOAc. The organic layer was washed with 1N HCl, H2O and dried over MgSO4. Solvent was evaporated under reduced pressure and the residue was purified by preparative TLC (Hexanes:EtOAc, 4:1) to afford the title compound as a white solid (107.3 mg). 1H NMR δ 3.54 (s, 1H), 3.60 (dd, 1H), 3.76 (dd, 1H), 5.12 (t, 1H), 7.45 (d, 2H), 8.14 (d, 2H); ESIMS: m/z 374 (M−H).

1. concentrationThe mixture was concentrated under reduced pressure
2. additiondiluted with EtOAc
3. washThe organic layer was washed with 1N HCl, H2O
4. dry with materialdried over MgSO4
5. customSolvent was evaporated under reduced pressure
6. customthe residue was purified by preparative TLC (Hexanes:EtOAc, 4:1)