反应详情

A solution of 200 μl of ethyloxalyl chloride in 1 ml of diethyl ether was added dropwise at 0° C. to a solution of 450 mg of 1c (contaminated with elimination products from previous reaction) and 200 μl of triethyl amine in 5 ml of ether. The reaction mixture was stirred for 20 min and then diluted with 10 ml of 1M K2CO3 and stirred for 5 min. The product was extracted with ethyl acetate and the extracts were washed once with water, dried and concentrated. The crude material was passed through a short silica column, using a gradient of heptane/ethyl acetate, as eluent, to provide 120 mg of 1d as colorless oil;

1. stirringstirred for 5 min
2. extractionThe product was extracted with ethyl acetate
3. washthe extracts were washed once with water
4. customdried
5. concentrationconcentrated