反应详情

A mixture of 7.67 g (0.0265 mole) of N-(1-methylethyl)-N-[2-(phenylsulfonyl)ethyl]carbamic chloride and 6.24 g (0.029 mole) of N'-[2-(diethylamino)ethyl]-N,N-diethyl-1,2-ethanediamine and 2.73 g (0.0270 mole) of triethylamine in 400 ml of tetrahydrofuran was refluxed for 6 hr and then was stirred at room temperature for 7 hr. The solvent was removed in vacuo and the residue was partitioned between methylene chloride and dilute sodium hydroxide. The methylene chloride solution was dried over sodium sulfate, and the solvent was removed in vacuo to give an oil. This was dissolved in ether, and the solution was extracted with three portions of water. The ether solution was dried over sodium sulfate, and the solvent was removed in vacuo to give an oil. This was pumped under high vacuum at 56° C. for 20 hr to give the title compound as an oil.

1. temperaturewas refluxed for 6 hr
2. customThe solvent was removed in vacuo
3. customthe residue was partitioned between methylene chloride and dilute sodium hydroxide
4. dry with materialThe methylene chloride solution was dried over sodium sulfate
5. customthe solvent was removed in vacuo
6. customto give an oil
7. extractionthe solution was extracted with three portions of water
8. dry with materialThe ether solution was dried over sodium sulfate
9. customthe solvent was removed in vacuo
10. customto give an oil
11. waitThis was pumped under high vacuum at 56° C. for 20 hr