반응 #806264
ord-a47443a3afa24c9d90c385c0cb0e18dd
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반응 조건
후처리
- 1기타The reaction
- 2여과was then filtered
- 3기타to give a colorless solution
- 4기타The solution was evaporated in vacuo
- 5기타leaving a damp, white solid
- 6여과The mixture was filtered
- 7기타resulting white solid
- 8세척was washed with pentane (3×3 mL)
- 9온도cooled to −35° C
- 10기타The white solid was dried in vacuo
- 11기타to yield 0.75 g (82%)
실험 절차
To a straw yellow solution of bis(propylcyclopentadienyl) zirconium dichloride [(PrCp)2ZrCl2] (1.00 g, 2.66 mmol, 1.00 eq.) in dichloromethane (10 mL) was added tributyltin fluoride (1.72 g, 5.57 mmol, 2.10 eq.). The reaction rapidly lightened, turning almost colorless. The reaction was stirred 1 h and was then filtered to give a colorless solution and a small amount of white solid. The solution was evaporated in vacuo, leaving a damp, white solid. Pentane (10 mL) was added and the mixture was cooled to −35° C. The mixture was filtered, and resulting white solid was washed with pentane (3×3 mL) cooled to −35° C. The white solid was dried in vacuo to yield 0.75 g (82%). 1H NMR(CD2Cl2): δ 0.92 (t, 6H, CH2CH2CH3), 1.56 (m, 4H, CH2CH2CH3), 2.44 (t, 4H, CH2CH2CH3), 6.05 (m, 4H, ring-H), 6.30 (m, 4H, ring-H). 19F NMR(CD2Cl2): δ 20.4 (s).