反応 #4314

反応方程式

N-[2-(phenylsulfonyl)ethyl]-2-propanamine

3-(N,N-diethylamino)propylisothiocyanate

→

white crystalline solid

収率 76.9%

N'-[3-(Diethylamino)propyl]-N-(1-methylethyl)-N-[2-(phenylsulfonyl)ethyl]thiourea

収率 76.9%

溶媒

acetonitrile

反応条件

後処理

1. 1
   その他The solvent was removed in vacuo
2. 2
   workup.DISSOLUTIONthe residue was dissolved in ether
3. 3
   抽出The solution was extracted with three portions of water
4. 4
   乾燥was dried over magnesium sulfate
5. 5
   workup.ADDITIONwas added until the solution
6. 6
   その他A white solid precipitated

実験手順

A solution of 5.0 g (0.022 mole) of N-[2-(phenylsulfonyl)ethyl]-2-propanamine and 4.30 g (0.025 mole) of 3-(N,N-diethylamino)propylisothiocyanate in 400 ml of acetonitrile was refluxed for 16 hr. The solvent was removed in vacuo and the residue was dissolved in ether. The solution was extracted with three portions of water and was dried over magnesium sulfate. The volume of the ether solution was reduced to 200 ml, and hexane was added until the solution became slightly cloudy. A white solid precipitated to give 6.76 g (76.9%) of white crystalline solid, m.p. 120°-121° C.

出典