反应详情

Acetoxyacetyl chloride (0.324 ml) is dropped into a solution of 4-amino-1-hydroxybutane-1,1-diphosphonic acid (500 mg) in water (5 ml) and1N NaOH (8 ml), simultaneously adding 1N NaOH (3 ml) to maintain pH between11 and 12. When the additions are completed, the reaction mixture is stirred at room temperature for 2 hours, then it is diluted with DMF: a precipitate separates which is recovered by centrifugation and purified byredissolution in water (3 ml) and reprecipitated with acetone (30 ml), to give 720 mg of N-(hydroxyacetyl)-4-amino-1-hydroxybutane-1,1-diphosphonic acid trisodium salt; m.p. >260°

1. temperatureto maintain pH between11 and 12
2. customa precipitate separates which is recovered by centrifugation
3. custompurified byredissolution in water (3 ml)
4. customreprecipitated with acetone (30 ml)