反応 #2787

反応方程式

water

imidazole

methyl 1-dimethoxyphosphinylethenesulfonate

bromotrimethylsilane

→

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

溶媒

chloroform

反応条件

後処理

1. 1
   workup.STIRRINGThe mixture is stirred for about 30 minutes
2. 2
   その他the layers are separated
3. 3
   抽出The water layer is extracted several times with CHCl3 (extracts are discarded)
4. 4
   その他is evaporated to dryness under vacuum
5. 5
   その他The residue is triturated with acetone
6. 6
   その他to give a solid, which
7. 7
   ろ過is collected by filtration
8. 8
   その他recrystallized from water/acetone

実験手順

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.

出典