反应详情

温度

0 °C

To a solution of tert-butyl 6-hydroxyhexylcarbamate (21 mmol) in CH2Cl2 (30 ml) was added imidazole (27 mmol) at 0° C. The reaction mixture was kept at 25° C. and stirred for 20 min, then cooled to 0° C. To the resulting reaction mixture was added tert-butyldimethylchlorosilane (23 mmol) dropwise over 30 min at 0° C. The reaction mixture was allowed to warm to 25° C. and stirred for 16 h and then filtered. The filtrate was washed with 1 N HCl (2×25 ml) and brine (30 ml), dried over Na2SO4, filtered and evaporated under reduced pressure. The residue was purified by SiO2 flash column (eluent: petroleum ether and then CH2Cl2). Yield 6.53 g (87% yield).

1. customwas kept at 25° C.
2. customTo the resulting reaction mixture
3. temperatureto warm to 25° C.
4. stirringstirred for 16 h
5. filtrationfiltered
6. washThe filtrate was washed with 1 N HCl (2×25 ml) and brine (30 ml)
7. dry with materialdried over Na2SO4
8. filtrationfiltered
9. customevaporated under reduced pressure
10. customThe residue was purified by SiO2 flash column (eluent