HRID7268

反应详情

EQUATION

反应方程式

HRID 7268 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 177 g of methanol, 43.7 g (0.216 mol) of 2,2,6,6-tetramethyl-3,5-heptanedione of 91% purity was dropwise added with stirring. To the resulting solution, a solution, which had been obtained by dissolving 12.7 g (0.054 mol) of ZrCl4 of 99% purity in 218 g of methanol and cooled to room temperature, was added over a period of about 5 minutes. The reaction was conducted for 1 hour with stirring, and 590 g of water was added over a period of 50 minutes. Then, stirring was performed for 1 hour. The resulting solution was adjusted to pH 6.6 with a 20% NaOH solution. The resulting crystals were collected by centrifugation and then dried. Thus, 43.9 g (yield: 98.2%) of tetrakis(2,2,6,6-tetramethyl-3,5-heptanedionato)zirconium was obtained.

WORKUP

后处理

  1. customTo the resulting solution, a solution, which had been obtained
  2. additionwas added over a period of about 5 minutes
  3. stirringwith stirring
  4. stirringThen, stirring
  5. waitwas performed for 1 hour
  6. customThe resulting crystals were collected by centrifugation
  7. customdried