تفاعل #4323

معادلة التفاعل

N,N-diethylethylenediamine

1,1'-carbonyldiimidazole

N-(2-propyl)-1-(phenylsulfonyl)-2-propanamine

→

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

المذيبات

tetrahydrofuran

tetrahydrofuran

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةthe solution was refluxed overnight
2. 2
   أخرىThe solvent was removed in vacuo
3. 3
   أخرىthe residue was partitioned between ether and water
4. 4
   تجفيفThe ether solution was dried over magnesium sulfate
5. 5
   أخرىthe solvent was removed in vacuo
6. 6
   أخرىto give an oil
7. 7
   أخرىchromatographed
8. 8
   غسيل(silica gel; elution with methanol)
9. 9
   أخرىto give an oil
10. 10
    أخرىCrystallization from ether
11. 11
    أخرىgave 0.54 g (4.5%) of white, crystalline solid, m.p. 75°-80° C.

الإجراء التجريبي

A solution of 3.71 g (0.032 mole) of N,N-diethylethylenediamine and 5.83 (0.036 mole) of 1,1'-carbonyldiimidazole in 400 ml of tetrahydrofuran was stirred at room temperature for 1 hr. A solution of 8.30 g (0.030 mole) of N-(2-propyl)-1-(phenylsulfonyl)-2-propanamine in 50 ml of tetrahydrofuran was added and the solution was refluxed overnight. The solvent was removed in vacuo, and the residue was partitioned between ether and water. The ether solution was dried over magnesium sulfate and the solvent was removed in vacuo to give an oil. The oil was flash chromatographed (silica gel; elution with methanol) to give an oil. Crystallization from ether gave 0.54 g (4.5%) of white, crystalline solid, m.p. 75°-80° C.

المصدر