反应详情

To a solution of 1-5 (19.3 g, 0.076 moles) in THF (400 ml)/H2O (195 ml) was added triphenylphosphine (80.0 g, 0.305 moles) in one portion at room temperature. This was stirred for 3 hours and the solvent was then removed in vacuo. The residue was acidified to pH 2 with 10% KHSO4 solution and this was extracted with 4×100 ml portions of EtOAc. The organic extract was extracted with 2×100 ml portions of 10% KHSO4 and the aqueous phases were combined and the pH was adjusted to pH 10 with 2N NaOH. This solution was extracted with EtOAc and the organic phase was dried (MgSO4), and the solvent was removed to give 1-6 as a yellow liquid, Rf 0.3 (silica gel 10% CH3OH in CHCl3 /NH3),

1. customthe solvent was then removed in vacuo
2. extractionthis was extracted with 4×100 ml portions of EtOAc
3. extractionThe organic extract
4. extractionwas extracted with 2×100 ml portions of 10% KHSO4
5. extractionThis solution was extracted with EtOAc
6. dry with materialthe organic phase was dried (MgSO4)
7. customthe solvent was removed