反应详情

温度

50 °C

210 mg of 2-dimethylaminoethanol were dissolved in 3 ml of dimethylformamide, and then 100 mg of a 50% w/w oily suspension of sodium hydride were added to the solution. This reaction mixture was then heated for 1 hour at 50° C. The reaction mixture was then cooled with ice, and a solution of 900 mg of 2-(3-iodopropyl)-5-methoxymethoxy-4,6,7-trimethyl-1,3-benzoxathiole (prepared as described in Example 86) in 2 ml of dimethylformamide was added dropwise, while stirring. After completion of the dropwise addition, the temperature of the reaction mixture was gradually raised, and then the mixture was heated for a further 2 hours at 50° C. The reaction mixture was then poured into water, and the resulting precipitate was extracted with benzene. The extract was washed with water and dried over anhydrous sodium sulfate. The benzene was distilled off under reduced pressure. The residual crude oily reaction product was separated by silica gel column chromatography. The fraction eluted with benzene was removed, while the fraction eluted with a 20:1 by volume mixture of ethyl acetate and triethylamine was subjected to silica gel Lobar column chromatography, eluted with the same eluent, to give the title compound.

1. additionwere added to the solution
2. temperatureThe reaction mixture was then cooled with ice
3. additionAfter completion of the dropwise addition
4. temperaturethe temperature of the reaction mixture was gradually raised
5. temperaturethe mixture was heated for a further 2 hours at 50° C
6. extractionthe resulting precipitate was extracted with benzene
7. washThe extract was washed with water
8. dry with materialdried over anhydrous sodium sulfate
9. distillationThe benzene was distilled off under reduced pressure
10. customThe residual crude oily reaction product was separated by silica gel column chromatography
11. washThe fraction eluted with benzene
12. customwas removed, while the fraction
13. washeluted with a 20:1 by volume mixture of ethyl acetate and triethylamine
14. washeluted with the same eluent