تفاعل #4324

معادلة التفاعل

N,N-diethyl-N'-methylethylenediamine

triethylamine

citric acid

N-(1-methylethyl)-N-[2-(phenylsulfonyl)ethyl]carbamic chloride

→

N-[2-(Diethylamino)ethyl]-N-methyl-N'-(1-methylethyl)-N'-[2-(phenylsulfonyl)ethyl]urea citrate hydrate

المذيبات

tetrahydrofuran

methanol

ether

ظروف التفاعل

المعالجة

1. 1
   أخرىThe solvent was removed in vacuo
2. 2
   workup.DISSOLUTIONthe residue was dissolved in a 60/40 mixture of ether and methylene chloride
3. 3
   استخلاصThis solution was extracted with several portions of water
4. 4
   تجفيفwas dried over magnesium sulfate
5. 5
   أخرىThe solvent was removed in vacuo
6. 6
   أخرىto give an oil
7. 7
   أخرىA solid precipitated
8. 8
   أخرىto give 11.08 g (82.4%) of white, crystalline solid

الإجراء التجريبي

A mixture of 6.65 g (0.023 mole) of N-(1-methylethyl)-N-[2-(phenylsulfonyl)ethyl]carbamic chloride; 3.0 g (0.023 mole) of N,N-diethyl-N'-methylethylenediamine and triethylamine (2.7 g, 0.0267 mole) in 400 ml of tetrahydrofuran was stirred at room temperature for 10 hr. The solvent was removed in vacuo, and the residue was dissolved in a 60/40 mixture of ether and methylene chloride. This solution was extracted with several portions of water and was dried over magnesium sulfate. The solvent was removed in vacuo to give an oil. This was dissolved in methanol, an excess of citric acid was added, and ether was added. A solid precipitated to give 11.08 g (82.4%) of white, crystalline solid; m.p. 77°-82° C.

المصدر