反应详情

温度

10 °C

A solution of 17.4 g (0.036 moles) of compound 19 in 100 ml of toluene was added over 10 min at 0° C. to a suspension of 8.5 g (0.036 moles) of 99.9% pure ZrCl4 in 100 ml of toluene. When the addition was complete, the reaction mixture was heated slowly to 10° C. over a period of 1 h and then stirred for 6 h at room temperature. The yellow precipitate was then filtered off, washed with 2×20 ml of toluene and 2×20 ml of hexane and dried under vacuum. The powder was purified further by removal of the residual tin compounds by means of extraction with refluxing toluene over a period of 3 h at 30 mm Hg and then with pentane over a period of 2 h in a Soxhlet extractor to leave 5.8 g (yield: 41%) of compound 20 in the form of a bright yellow powder. No 1H NMR was obtained because of the insolubility of this compound.

1. additionWhen the addition
2. filtrationThe yellow precipitate was then filtered off
3. washwashed with 2×20 ml of toluene and 2×20 ml of hexane
4. customdried under vacuum
5. customThe powder was purified further by removal of the residual tin compounds by means of extraction with refluxing toluene over a period of 3 h at 30 mm Hg