反应详情

Water (173 ml) and sodium carbonate (33.24 g, 310 mM) were added to a stirred ethereal solution (123 ml) of 6-amino-2-bromo-4-chloro-phenol (17.45 g, 78.4 mM). After 15 minutes 3,5-di-t-butyl-4-hydroxy-phenylacetyl chloride (47.60 g, 93.1%, 156.8 mM) (prepared with thionyl chloride from the corresponding acid), was added at -5° to 0° C. and stirring continued for a further 1.5 hours without cooling. The aqueous phase was adjusted to pH 8 and the layers separated. The organics were washed with 1N HCl (100 ml) and saturated aqueous sodium bicarbonate solution (100 ml), dried (Na2SO4) and evaporated in-vacuo to give 58.1 g (103.6%) of the title compound which was suitable for the next step.

1. additionwas added at -5° to 0° C.
2. temperaturewithout cooling
3. customthe layers separated
4. washThe organics were washed with 1N HCl (100 ml) and saturated aqueous sodium bicarbonate solution (100 ml)
5. dry with materialdried (Na2SO4)
6. customevaporated in-vacuo