反応 #806263

反応方程式

Pentane

tributyltin fluoride

(tetramethylcyclopentadienyl)(propylcyclopentadienyl) zirconium dichloride

tributyltin fluoride

→

(tetramethylcyclopentadienyl)(propylcyclopentadienyl) zirconium difluoride

溶媒

dichloromethane

反応条件

後処理

1. 1
   その他The reaction
2. 2
   ろ過was then filtered
3. 3
   その他to give a colorless solution
4. 4
   その他The solution was evaporated in vacuo
5. 5
   その他leaving a damp, white solid
6. 6
   ろ過The mixture was filtered
7. 7
   その他resulting white solid
8. 8
   洗浄was washed with pentane (3×3 mL)
9. 9
   温度cooled to −35° C
10. 10
    その他The white solid was dried in vacuo
11. 11
    その他to yield 0.88 g (96%)

実験手順

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).

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