반응 #4324

반응 방정식

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

용매

tetrahydrofuran

methanol

ether

반응 조건

후처리

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

실험 절차

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.

출처