反应详情

温度

0 °C

(2-Cyclohexa-1,3-dienyl-ethoxymethyl)-benzene (9) (6 g, 28 mmol) is dissolved in 280 ml of dry methylene chloride and cooled down to 0° C. After addition of molecular sieves (6 g, UOP Type 4A) and N—BOC-hydroxylamine (5.6 g, 42 mmol) in small portions, tetrapropylammonium(meta)periodate (10.8 g, 28 mmol) is added slowly in small portions the mixture was stirred for 1 h. Then the mixture is diluted with CH2C12 and cooled to −10° C. 2M Na2S2O5 solution is added slowly (exothermic!). The mixture is washed with water, dried over Na2SO4 and evaporated under reduced pressure. The crude product is purified by Flash-chromatography (ethyl acetate/hexanes (1:9), silicagel).

1. additionis added slowly in small portions the mixture
2. additionThen the mixture is diluted with CH2C12
3. temperaturecooled to −10° C
4. washThe mixture is washed with water
5. dry with materialdried over Na2SO4
6. customevaporated under reduced pressure
7. customThe crude product is purified by Flash-chromatography (ethyl acetate/hexanes (1:9), silicagel)