反应详情

To a solution of 0.95 g (4.0 mmol) 2-(4-hydroxy-2-methyl-phenoxy)-2-methyl-propionic acid ethyl ester (described in WO 02/092590) and 0.42 ml (4.0 mmol) 5-chloro-pent-1-yne in 20 ml acetonitrile were added 0.60 g (4.0 mmol) NaI and 1.56 g (4.80 mmol) Cs2CO3. The mixture was stirred at 50° C. for 3 days and every day 0.42 ml (4.0 mmol) 5-chloro-pent-1-yne and 1.56 g (4.80 mmol) Cs2CO3 were added (two times). After 2 further days stirring at ambient temperature and filtration, the solvent was evaporated. The residue was redissolved in dichloromethane, dried (Na2SO4), filtered and evaporated. Purification by flash chromatography (SiO2, n-heptane/EtOAc 2.5 to 5%) yielded 1.11 g of the title compound as colorless oil.

1. additionwere added (two times)
2. filtrationfiltration
3. customthe solvent was evaporated
4. dissolutionThe residue was redissolved in dichloromethane
5. dry with materialdried (Na2SO4)
6. filtrationfiltered
7. customevaporated
8. customPurification by flash chromatography (SiO2, n-heptane/EtOAc 2.5 to 5%)