Synthesis of High-Purity Diorganozinc Compounds for Coordinative Chain Transfer Polymerization
- 주제(키워드) Diorganozinc compounds , Coordinative Chain Transfer Polymerization , High purity , Industrial feasibility
- 주제(DDC) 547
- 발행기관 아주대학교 일반대학원
- 지도교수 이분열
- 발행년도 2026
- 학위수여년월 2026. 2
- 학위명 석사
- 학과 및 전공 일반대학원 분자과학기술학과
- 실제URI http://www.dcollection.net/handler/ajou/000000035423
- 본문언어 영어
- 저작권 아주대학교 논문은 저작권에 의해 보호받습니다.
초록/요약
Diorganozinc compounds (R₂Zn) are versatile reagents that are widely used in organic synthesis and as chain-transfer agents in Coordinative Chain Transfer Polymerization (CCTP). However, conventional synthesis using ZnCl₂ and Grignard reagents (RMgX) often produces R₂Zn containing Cl⁻ and Mg2+ impurities, which deactivate CCTP catalysts. Purification using vacuum distillation or treatment with n-BuLi-modified silica removes these impurities, but involve hazardous conditions and are unsuitable for large-scale production. In this study, a facile one- filtration process was developed to safely and efficiently synthesize high-purity R₂Zn compounds. Rapid injection of ZnCl₂ solution into RMgX induces instantaneous reflux, and residual MgCl₂ functions as an active scavenger to eliminate salt-type impurities. The use of diethyl ether or dimethoxymethane (methylal) as the solvent, provided 96–98% yield of R₂Zn with Cl < 5 ppm, Mg = 3–4 ppm, and reproducibly on a 1–100 g scale. This method was successfully applied to various R₂Zn derivatives showing high activity in CCTP. This study provides a scalable and practical route for producing high-purity R₂Zn, which would contribute to the implementation of CCTP technology.
more목차
1. Introduction 1
2. Results and Discussion 6
2.1. Direct synthesis of R₂Zn suitable for CCTP applications 6
2.2. CCTP Performance of Synthesized R2Zn Compounds 13
3. Conclusion. 15
4. Experimental Section 16
4.1. General remarks 16
4.2. Synthesis of (CH₂=CHC₆H₄CH₂CH₂CH₂)₂Zn 16
4.3. Large scale synthesis of (CH₂=CHC₆H₄CH₂CH₂CH₂)₂Zn 17
5. Reference 19
6. Supporting information 23
