反应详情

MS: M=304.2(API+). 1H-NMR(400 MHz, D6-DMSO): δ=4.71(s, 2H, CH2Cl), 7.21(d, 1H, ═CH), 7.40(d, 2H, Ar—H), 7.58(d, 1H, ═CH), 7.87(d, 2H, Ar—H), 8.19(s, 1H, oxazole). 0.304 g (1.00 mmol) 4-Chloromethyl-2-[2-(4-trifluoromethoxy-phenyl)-vinyl]-oxazole, 0.217 g (1.00 mmol) 4-(4-[1,2,3]Triazol-1-yl-butyl)-phenol, 0.166 g (1.00 mmol) potassium iodide and 0.191 ml (1.00 mmol) of a 30% sodium methylate solution were added to 50.0 ml methanol and heated to reflux for 8 h. After removal of solvent, partitioning of the residue between 50 ml ethyl acetate and 15 ml water, the organic phase was washed with 10 ml water, 10 ml 0.1 N NaOH, 15 ml water twice and dried over sodium sulphate. The solution was concentrated until crystallisation of the product started. After leaving for 1 h at room temperature the precipitate was isolated, washed with ether and dried at 40° C. in vacuo. Yield 0.16 g (32%) 2, m.p. 138–140° C.

1. temperatureheated
2. temperatureto reflux for 8 h
3. customAfter removal of solvent
4. custompartitioning of the residue between 50 ml ethyl acetate and 15 ml water
5. washthe organic phase was washed with 10 ml water, 10 ml 0.1 N NaOH, 15 ml water twice
6. dry with materialdried over sodium sulphate
7. concentrationThe solution was concentrated until crystallisation of the product
8. customAfter leaving for 1 h at room temperature the precipitate
9. customwas isolated
10. washwashed with ether
11. customdried at 40° C. in vacuo