反应详情

[2-(2,6-Dichloro-phenyl)-ethyl]-(3-iodo-benzyl)-carbamic acid tert-butyl ester (506 mg), tetrabutylammonium chloride (280 mg), sodium bicarbonate (210 mg), allyl alcohol (100 μL) and toluene (20 mL) were charged to a flask, followed by palladium acetate (10 mg) and the resultant mixture heated to 80° C., under nitrogen for 5 hours. On cooling, the reaction was filtered, the filtrate diluted with toluene and extracted sequentially, twice with water, once with brine, dried (magnesium sulfate) and evaporated. Purification on silica, eluting with a gradient of iso-hexane/ethyl acetate [4:1 to 2:1], gave the subtitle product as an oil (300 mg).

1. temperatureOn cooling
2. filtrationthe reaction was filtered
3. additionthe filtrate diluted with toluene
4. extractionextracted sequentially, twice with water, once with brine
5. dry with materialdried (magnesium sulfate)
6. customevaporated
7. customPurification on silica
8. washeluting with a gradient of iso-hexane/ethyl acetate [4:1 to 2:1]