反应详情

200 g of 2-(3-carbamoylphenylamino)-N-(3,4-dimethoxyphenethyl)acetamide trihydrate and 65.2 g of sodium hydroxymethanesulfonate were suspended in 400 ml of water, and the suspension was refluxed over night. After cooling, the reaction mixture was washed with chloroform, and an insoluble material was removed by filtration. The filtrate was concentrated in vacuo. The residue was dissolved in a mixture of 500 ml of water and 500 ml of ethanol under heating, and then the solution was cooled. The precipitate formed was collected by filtration and recrystallized from a mixture of water and ethanol to give 59.2 g of sodium N-(3-carbamoylphenyl)-N-(2-((2-(3,4-dimethoxyphenyl)ethyl)amino)-2-oxoethyl)aminomethanesulfonate dihydrate as colorless crystals with m.p. 253° to 255° C. (decomposition).

1. temperaturethe suspension was refluxed over night
2. temperatureAfter cooling
3. washthe reaction mixture was washed with chloroform
4. customan insoluble material was removed by filtration
5. concentrationThe filtrate was concentrated in vacuo
6. dissolutionThe residue was dissolved in a mixture of 500 ml of water and 500 ml of ethanol
7. temperatureunder heating
8. temperaturethe solution was cooled
9. customThe precipitate formed
10. filtrationwas collected by filtration
11. customrecrystallized from a mixture of water and ethanol