HRID1778454

反应详情

EQUATION

反应方程式

HRID 1778454 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a light yellow solution of chlorodimethyl(2-methyl-4-phenyl-1H-indenyl)silane (9.40 g, 31.4 mmol, 1.00 eq.) in tetrahydrofuran (40 ml) at −30° C. was added sodium (tetramethylcyclopentadienide) (4.76 g, 33.0 mmol, 1.05 equiv.) in portions to give a cloudy orange solution. The reaction was allowed to warm to room temperature and stirred for 23 hours. The mixture was evaporated under vacuum, leaving an orange residue. The residue was extracted with pentane (50 ml) and the extract was filtered to give a bright yellow solution and yellow solid. The solution was evaporated under vacuum to yield thick, orange oil. Yield 10.16 g (84%). 1H NMR(C6D6): δ7.61 (d, 2H), 7.41 (m, 1H), 7.31 (m, 4H), 7.19 (m, 1H), 6.85 (s, 1H), 3.60, (s, 1H), 3.16 (br s, 1H), 2.00 (s, 3H), 1.93 (s, 3H), 1.88 (s, 3H), 1.82 (s, 6H), −0.23 (s, 3H), −0.24 (s, 3H).

WORKUP

后处理

  1. customto give a cloudy orange solution
  2. customThe mixture was evaporated under vacuum
  3. customleaving an orange residue
  4. extractionThe residue was extracted with pentane (50 ml)
  5. filtrationthe extract was filtered
  6. customto give a bright yellow solution and yellow solid
  7. customThe solution was evaporated under vacuum
  8. customto yield thick