반응 #4322

반응 방정식

1-(3-aminopropyl)-4-methylpiperazine

1,1'-carbonyldiimidazole

maleic acid

N-(2-phenylsulfonylethyl)-2-propanamine

→

white crystalline solid

수율 68.8%

N-(1-Methylethyl)-N'-[3-(4-methyl-1-piperazinyl)propyl]-N-[2-(phenylsulfonyl)ethyl]urea maleate

수율 68.8%

용매

tetrahydrofuran

methanol

methanol

tetrahydrofuran

반응 조건

후처리

1. 1
   온도the mixture was refluxed for 16 hr
2. 2
   기타The solvent was removed in vacuo
3. 3
   기타the residue was partitioned between methylene chloride and water
4. 4
   건조The solution was dried over magnesium sulfate
5. 5
   기타the solvent was removed in vacuo
6. 6
   기타to give an oil
7. 7
   기타a white solid precipitated
8. 8
   기타This was collected

실험 절차

A mixture of 6.00 g (0.035 mole) of 1-(3-aminopropyl)-4-methylpiperazine and 6.97 g (0.043 mole) of 1,1'-carbonyldiimidazole in 400 ml of tetrahydrofuran was stirred at room temperature for 1 hr. A solution of 8.17 g (0.036 mole) of N-(2-phenylsulfonylethyl)-2-propanamine in 100 ml of tetrahydrofuran was added, and the mixture was refluxed for 16 hr. The solvent was removed in vacuo and the residue was partitioned between methylene chloride and water. The solution was dried over magnesium sulfate, and the solvent was removed in vacuo to give an oil. The oil was dissolved in methanol; a solution of two equivalents of maleic acid in methanol was added, and a white solid precipitated. This was collected to give 15.48 g (68.8%) of white crystalline solid; m.p. 162°-163° C. with decomposition.

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