反应详情

15 g of tetraethyleneglycol and 23.4 g of triethylamine were dissolved in 200 mL of dichloromethane, to which 22.1 g of methanesulfonylchloride was added dropwise at 0° C., and then the solution was stirred for 1 hour. The reaction solution was filtrated to remove insolubles, and then the filtrate was concentrated under reduced pressure. The residue was separated with ethyl acetate-water, and the organic layer was concentrated under reduced pressure after washing with water. The residue was purified with silica gel column chromatography to obtain 27 g of the objective compound.

1. additionwas added dropwise at 0° C.
2. filtrationThe reaction solution was filtrated
3. customto remove insolubles
4. concentrationthe filtrate was concentrated under reduced pressure
5. customThe residue was separated with ethyl acetate-water
6. concentrationthe organic layer was concentrated under reduced pressure
7. washafter washing with water
8. customThe residue was purified with silica gel column chromatography