反应详情

温度

-78 °C

11.4 g (0.052 mole) of compound 2 and 100 ml methylene chloride (CH2Cl2) were placed in a 250 ml Schlenk tube. These solution was cooled to −78° C. and 9.8 g (5.6 ml, 0.052 mole) titanium tetrachloride were added drop-wise over 10 minutes. The red solution obtained was slowly heated to room temperature and was stirred for a further 3 hours. The solvent was removed under vacuum, whereupon a yellowish product was obtained. 200 ml hexane were added to the crude solid, and yellow solution obtained was filtered and cooled overnight in a refrigerator, whereupon 12.3 g (79% of the theoretical yield) of yellow crystals of compound 3 were obtained. It should be mentioned that in J. Organometallic Chem. 169 (1979), 373, 62% of the theoretical yield was obtained when the reaction was conducted in a hydrocarbon solvent such as petroleum ether or methylcyclohexane.

1. customThe red solution obtained
2. temperaturewas slowly heated to room temperature
3. customThe solvent was removed under vacuum, whereupon a yellowish product
4. customwas obtained
5. customobtained
6. filtrationwas filtered
7. temperaturecooled overnight in a refrigerator, whereupon 12.3 g (79% of the