反应详情

Subsequently, 1.0 l of tetrahydrofuran and 750 g (3.29 mol) of acetylferrocene (dried overnight at 40° C. in vacuo) were added to the catalyst solution thus obtained and dissolved by further addition of 1.0 l of tetrahydrofuran. The amount of catalyst was thus 6.8 mol%. At 20°-25° C., a further 145 ml of borane-dimethyl sulphide adduct (1.75 mol altogether) was added dropwise and uniformly over a period of 3 hours. After stirring for a further 30 minutes, the reaction mixture was hydrolysed while cooling by addition of 2.0 l of water, with care being taken to ensure that the temperature did not rise above 30° C. Subsequently, 2.0 l of tert-butyl methyl ether were added, the phases were separated and the aqueous phase was extracted once more with 1.0 l of tert-butyl methyl ether. The combined organic phases were dried over magnesium sulphate and the solvent was distilled off.

1. customthus obtained
2. customdid not rise above 30° C
3. customthe phases were separated
4. extractionthe aqueous phase was extracted once more with 1.0 l of tert-butyl methyl ether
5. dry with materialThe combined organic phases were dried over magnesium sulphate
6. distillationthe solvent was distilled off