反应详情

To a flask under argon containing 4.94 g (0.0119 mole) diltiazem was added 50 ml ethyl acetate and 3.48 g (0.0119 mole) 3,4-dimethoxyphenethyl iodide. The reaction was refluxed for 24 hr then filtered. The filtrate was washed with sodium bicarbonate and brine, dried over K2CO3, and 0.85 g 3,4-dimethoxyphenethyl iodide added and the reaction refluxed for 18 hr then filtered. The last step was repeated but 1.75 g of 3,4-dimethoxyphenethyl iodide was added and the reaction refluxed 5 hr. The filtered materials were combined and recrystallized from 95% ethanol to give a mixture of product and diltiazem hydroiodide.

1. temperatureThe reaction was refluxed for 24 hr
2. filtrationthen filtered
3. washThe filtrate was washed with sodium bicarbonate and brine
4. dry with materialdried over K2CO3, and 0.85 g 3,4-dimethoxyphenethyl iodide
5. additionadded
6. temperaturethe reaction refluxed for 18 hr
7. filtrationthen filtered
8. addition1.75 g of 3,4-dimethoxyphenethyl iodide was added
9. temperaturethe reaction refluxed 5 hr
10. customrecrystallized from 95% ethanol
11. customto give