反应详情

To a stirring solution of 44 (1.5 g, 6.6 mmol), imidazole (1.13 g, 16.6 mmol, 2.5 equ) and triphenylphosphine (4.40 g, 16.8 mmol, 2.5 equ) in toluene (250 ml) under nitrogen was added iodine (3.26 g, 12.8 mmol, 1.9 equ). The reaction mixture was stirred for one hour then filtered. The filtrate was washed with 8% sodium thiosulphate solution (250 ml) and brine (100 ml) then dried (Na2SO4) and concentrated in vacuo to give a white solid. This solid was taken up in hexane, cooled and filtered. The filtrate was then concentrated in vacuo to give 46 (1.1 g, 61%) as a colourless oil.

1. filtrationthen filtered
2. washThe filtrate was washed with 8% sodium thiosulphate solution (250 ml) and brine (100 ml)
3. dry with materialthen dried (Na2SO4)
4. concentrationconcentrated in vacuo
5. customto give a white solid
6. temperaturecooled
7. filtrationfiltered
8. concentrationThe filtrate was then concentrated in vacuo