HRID614224

反应详情

EQUATION

反应方程式

HRID 614224 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

18.8 g (0.05 mol) of the ethyl-1-[(1,2,2,6,6-pentamethyl-4-piperidyl)-amino]-n-heptyl-phosphonate from Example 2 are dissolved in 400 ml of ethanol with the addition of 3.40 g (0.05 mol) of sodium ethylate. A solution of 4.14 g (0.025 mol) of nickel chloride dihydrate in 100 ml of ethanol is added dropwise to this solution at 25° and the mixture is stirred at 25° for 3 hours. The sodium chloride which has precipitated out is now filtered off, the solvent is evaporated off and the residue is extracted with ether. After volatilising the solvent, the extract is dried for 10 hours at a temperature of 60° and under a pressure of 11 mm Hg. Ni-di-{ethyl-1-[(1,2,2,6,6-pentamethyl-4-piperidyl)-amino]-n-heptyl-phosphonate}-monohydrate is obtained as a green-yellow solid product. It is soluble in hexane at room temperature.

WORKUP

后处理

  1. customThe sodium chloride which has precipitated out
  2. filtrationis now filtered off
  3. customthe solvent is evaporated off
  4. extractionthe residue is extracted with ether
  5. customthe extract is dried for 10 hours at a temperature of 60° and under a pressure of 11 mm Hg