反応 #4321

反応方程式

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

2-phenylsulfonylethanamine

1,1'-carbonyldiimidazole

→

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

溶媒

tetrahydrofuran

tetrahydrofuran

反応条件

後処理

1. 1
   温度the mixture was refluxed for 13 hr
2. 2
   その他The solvent was removed in vacuo
3. 3
   workup.DISSOLUTIONthe residue was dissolved in a 50/50 mixture of ether and methylene chloride
4. 4
   抽出The solution was extracted with water
5. 5
   乾燥was dried over magnesium sulfate
6. 6
   その他The solvent was removed in vacuo
7. 7
   その他in give an oil
8. 8
   その他Flash chromatography on silica gel (methanol) gave 5.74 g (41.36%) of clear, colorless oil

実験手順

A mixture of 6.96 g (0.0376 mole) of 2-phenylsulfonylethanamine and 6.64 g (0.041 mole) of 1,1'-carbonyldiimidazole in 400 ml of tetrahydrofuran was stirred at room temperature for 1 hr. A solution of 6.16 g (0.039 mole) of N-[2-(diethylamino)ethyl]-2-propanamine in 50 ml of tetrahydrofuran was added, and the mixture was refluxed for 13 hr. The solvent was removed in vacuo, and the residue was dissolved in a 50/50 mixture of ether and methylene chloride. The solution was extracted with water and was dried over magnesium sulfate. The solvent was removed in vacuo in give an oil. Flash chromatography on silica gel (methanol) gave 5.74 g (41.36%) of clear, colorless oil:

出典