HRID1348537

反应详情

EQUATION

反应方程式

HRID 1348537 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 3.52 g (10 mmol) of an adduct of cyclopentadienyl zirconium trichloride with dimethoxyethane in toluene, a suspension of 2.2 g (10 mmol) of potassium (2-trimethylsiloxy-ethyl)-cyclopentadienide in toluene is added. The addition is carried out at −78° C. An orange-brown suspension is immediately formed; it is maintained under stirring for 12 hours; then it is left settling and it is filtered. The obtained orange solution is concentrated up to 5 ml and hexane is added, so that a brown solid is obtained. (1.1 g, 2.7 mmol. Yield: 27%). 1H-NMR: 6.00 (t, 2H), 5.87 (s, 5H), 5.67 (t, 2H), 3.66 (t, 2H), 2.92 (t, 2H), 0.11 (s, 9H). Mass spectrum. M+-65: (343): 33%.

WORKUP

后处理

  1. additionis added
  2. additionThe addition
  3. customis carried out at −78° C
  4. customAn orange-brown suspension is immediately formed
  5. temperatureit is maintained
  6. waitthen it is left
  7. filtrationit is filtered
  8. concentrationThe obtained orange solution is concentrated up to 5 ml and hexane
  9. additionis added, so that a brown solid
  10. customis obtained