HRID1977

反应详情

EQUATION

反应方程式

HRID 1977 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

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.

WORKUP

后处理

  1. concentrationthe mixture was concentrated under vacuum
  2. additionTo the residue was added 3N NH4OH (8 mL) which
  3. customThe solvent was removed in vacuo
  4. concentrationthe residue concentrated from methanol (2 mL)