반응 #2787

반응 방정식

water

imidazole

methyl 1-dimethoxyphosphinylethenesulfonate

bromotrimethylsilane

→

2-(1-imidazolyl)-1-phosphonoethanesulfonic acid

용매

chloroform

반응 조건

후처리

1. 1
   workup.STIRRINGThe mixture is stirred for about 30 minutes
2. 2
   기타the layers are separated
3. 3
   추출The water layer is extracted several times with CHCl3 (extracts are discarded)
4. 4
   기타is evaporated to dryness under vacuum
5. 5
   기타The residue is triturated with acetone
6. 6
   기타to give a solid, which
7. 7
   여과is collected by filtration
8. 8
   기타recrystallized from water/acetone

실험 절차

A mixture of 0.68 g (0.01 mole) of imidazole and 2.30 g (0.01 mole) of methyl 1-dimethoxyphosphinylethenesulfonate (U.S. Pat. No. 5,011,938 issued to Barnett et al. on Apr. 30, 1991) in 20 ml of chloroform is stirred at 20°-50° for one day. The reaction is cooled to room temperature, and 10.7 g (0.07 mole) of bromotrimethylsilane is added. The mixture is stirred at 20°-30° for 2-3 days, and to it is then added 20 ml water. The mixture is stirred for about 30 minutes, and the layers are separated. The water layer is extracted several times with CHCl3 (extracts are discarded) and is evaporated to dryness under vacuum. The residue is triturated with acetone to give a solid, which is collected by filtration and recrystallized from water/acetone to afford 2-(1-imidazolyl)-1-phosphonoethanesulfonic acid.

출처