반응 #56118

반응 방정식

thionyl chloride

1-(2',6'-dichlorophenyl)-2-(2',3'-bismethoxycarbonylguanidino) ethanol

sodium hydroxide

methyl alcohol

→

4,5-Dihydro-2-methoxycarbonylamino-5-(2',6'-dichlorophenyl)imidazole

용매

methylene chloride

water

반응 조건

후처리

1. 1
   workup.ADDITIONwas added dropwise
2. 2
   workup.ADDITIONAt the conclusion of the addition period
3. 3
   온도the resulting mixture refluxed for 60 minutes
4. 4
   기타The reaction solution was evaporated to low volume under vacuum and 50 ml of water
5. 5
   workup.ADDITIONadded
6. 6
   기타The precipitated solid was collected
7. 7
   세척washed with methanol
8. 8
   기타dried

실험 절차

To 1 gram of 1-(2',6'-dichlorophenyl)-2-(2',3'-bismethoxycarbonylguanidino) ethanol dissolved in 20 ml of methylene chloride was added dropwise with cooling at 0° C. 0.35 g of thionyl chloride. At the conclusion of the addition period, the solution was stirred for an additional 60 minutes at room temperature. After the addition of 20 ml of methyl alcohol, a solution of 0.5 g of sodium hydroxide in 2 ml of water was added and the resulting mixture refluxed for 60 minutes. The reaction solution was evaporated to low volume under vacuum and 50 ml of water added. The precipitated solid was collected, washed with methanol, followed by water and dried. 4,5-Dihydro-2-methoxycarbonylamino-5-(2',6'-dichlorophenyl)imidazole was isolated, 0.3 g, m.p. 229-230 (dec.).

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