反应详情

A degassed (argon) solution of 0.098 g (0.44 mmol) 1-fluoro-3-iodobenzene in 4 ml acetonitrile was treated with 0.111 g (0.40 mmol) 2-methyl-2-(2-methyl-4-pent-4-ynyloxy-phenoxy)-propionic acid (example 26B]), 0.014 g (0.02 mmol) PdCl2(Ph3P)2, 0.004 g (0.02 mmol) of CuI and 0.17 ml (1.20 mmol) triethylamine. The reaction was stirred for 2.5 h and then extracted with chilled aqueous 10% KHSO4/ether (three times). The organic phases were washed with aqueous 10% NaCl, dried (Na2SO4) and evaporated. Purification was done by flash-chromatography on silica gel (1. n-heptane/EtOAc 4:1 and 2. CH2Cl2/MeOH 2%-10%). The pure fractions were evaporated, dissolved in ether and washed with aqueous 10% KHSO4/ether (three times). The organic phase was dried (Na2SO4) and evaporated to yield 0.10 g of the title compound as an orange viscous oil.

1. extractionextracted with chilled aqueous 10% KHSO4/ether (three times)
2. washThe organic phases were washed with aqueous 10% NaCl
3. dry with materialdried (Na2SO4)
4. customevaporated
5. customPurification
6. customThe pure fractions were evaporated
7. dissolutiondissolved in ether
8. washwashed with aqueous 10% KHSO4/ether (three times)
9. dry with materialThe organic phase was dried (Na2SO4)
10. customevaporated