反应详情

温度

160 °C

35 g of the product of Example 24 were dissolved in 75 ml of dimethylformamide, and 10.5 g of copper(I) cyanide were added. The mixture was stirred for 8 hours at 160° C. The hot mixture was then discharged into 100 ml of ice-water, and 30 g of 1,2-diaminoethane were added. After stirring for 30 minutes, the organic phase was separated off and the aqueous phase was extracted with methylene chloride. The combined organic phases were washed with a solution of 30 g of 1,2-diaminoethane in 75 ml of water, dried over magnesium sulphate and distilled under high vacuum to give 20.5 g of product (=69% of theory). The. boiling point was 110° C. at 0.02 mbar. =19F NMR: -58.1 and -84.6 ppm. 1H NMR: 3.08 ppm.

1. additionwere added
2. stirringAfter stirring for 30 minutes
3. customthe organic phase was separated off
4. extractionthe aqueous phase was extracted with methylene chloride
5. washThe combined organic phases were washed with a solution of 30 g of 1,2-diaminoethane in 75 ml of water
6. dry with materialdried over magnesium sulphate
7. distillationdistilled under high vacuum