반응 #806263

반응 방정식

Pentane

tributyltin fluoride

(tetramethylcyclopentadienyl)(propylcyclopentadienyl) zirconium dichloride

tributyltin fluoride

→

(tetramethylcyclopentadienyl)(propylcyclopentadienyl) zirconium difluoride

용매

dichloromethane

반응 조건

후처리

1. 1
   기타The reaction
2. 2
   여과was then filtered
3. 3
   기타to give a colorless solution
4. 4
   기타The solution was evaporated in vacuo
5. 5
   기타leaving a damp, white solid
6. 6
   여과The mixture was filtered
7. 7
   기타resulting white solid
8. 8
   세척was washed with pentane (3×3 mL)
9. 9
   온도cooled to −35° C
10. 10
    기타The white solid was dried in vacuo
11. 11
    기타to yield 0.88 g (96%)

실험 절차

To a yellow solution of (tetramethylcyclopentadienyl)(propylcyclopentadienyl) zirconium dichloride [(Me4Cp)(PrCp)ZrCl2] (1.00 g, 2.47 mmol, 1.00 eq.) in dichloromethane (10 mL) was added tributyltin fluoride (1.60 g, 5.18 mmol, 2.09 eq.). The reaction quickly lightened, becoming almost colorless with a small amount of tributyltin fluoride still visible. 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 (15 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 0.88 g (96%). 1H NMR(CD2Cl2): δ 0.92 (t, 3H, CH2CH2CH3), 1.55 (m, 2H, CH2CH2CH3), 1.82 (s, 6H, Me), 1.99 (s, 6H, Me), 2.42 (t, 2H, CH2CH2CH3), 5.93 (s, 1H, ring-H), 5.96 (br m, 2H, ring-H), 6.17 (m, 2H, ring-H). 19F NMR(CD2Cl2): δ 17.5 (s).

출처