반응 #2073

반응 방정식

tetraethyl 3-aminooctane-1,1-bisphosphonate

bromotrimethylsilane

→

3-aminooctane-1,1-bisphosphonic acid, triammonium salt

용매

dichloromethane

반응 조건

후처리

1. 1
   농축the mixture was concentrated under vacuum
2. 2
   workup.ADDITIONTo the residue was added 3N NH4OH (8 mL) which
3. 3
   기타The solvent was removed in vacuo
4. 4
   농축the residue concentrated from methanol (2 mL)

실험 절차

To a solution of tetraethyl 3-aminooctane-1,1-bisphosphonate (0.45 g, 1.12 mmol) in dry dichloromethane (1.1 mL) was added bromotrimethylsilane (1.05 mL, 7.85 mmol) via syringe. After 18 hours, the mixture was concentrated under vacuum. To the residue was added 3N NH4OH (8 mL) which was stirred for 30 minutes at room temperature. The solvent was removed in vacuo and the residue concentrated from methanol (2 mL) to give 0.40 g of 3-aminooctane-1,1-bisphosphonic acid, triammonium salt as a white powder.

출처