反应详情

温度

130 °C

A mixture of 26.5 g (71.8 mmol) (6-chloro-4-iodo-pyridin-3-yl)-methyl-carbamic acid tert-butyl ester and 25.4 g (144 mmol) (2S,4R)-2-(hydroxymethyl)-4-hydroxypyrrolidine in 260 ml dimethyl sulfoxide was stirred at 130° C. for 32 h. The reaction mixture was concentrated in vacuo, treated with 200 ml 2 N sodium carbonate solution and extracted with three 200-ml portions of ethyl acetate. The organic layers were washed with 200 ml 2 N sodium carbonate solution and 200 ml brine and dried over sodium sulfate. Flash chromatography gave 15.5 g (48%) of the title compound as a white foam.

1. concentrationThe reaction mixture was concentrated in vacuo
2. additiontreated with 200 ml 2 N sodium carbonate solution
3. extractionextracted with three 200-ml portions of ethyl acetate
4. washThe organic layers were washed with 200 ml 2 N sodium carbonate solution and 200 ml brine
5. dry with materialdried over sodium sulfate