反应详情

A solution of 5.5 g (30 mmoles) of dimethyl azodicarboxylate is added dropwise, at room temperature, to a solution of 5.8 g (20 mmoles) of 2-(2,4-dichlorophenyl)-2-isopropoxypentan-1-ol, 7.9 g (30 mmoles) of triphenylphosphine and 1.66 g (24 mmoles) of 1,2,4-triazole in 100 ml of absolute tetrahydrofuran, and the reaction mixture is then stirred for 3 hours at room temperature and then for a further 16 hours at 50° C. and is evaporated; the residue is digested with 100 ml of diethyl ether, the insoluble residue is filtered off, and the ether phase is concentrated again and purified by column chromatography (silica gel; 1:1 ethyl acetate/petroleum ether). This gives a colourless oil having physical data which agree entirely with those in Example 3b).

1. waitfor a further 16 hours at 50° C.
2. customis evaporated
3. filtrationthe insoluble residue is filtered off
4. concentrationthe ether phase is concentrated again
5. custompurified by column chromatography (silica gel; 1:1 ethyl acetate/petroleum ether)
6. customThis gives a colourless oil