反应详情

To a suspension of 22 g (0.1 mole) of chromium hexacarbonyl in ether is slowly added phenyllithium (51 ml, 0.1 mole, cyclohexane:ether solution) via syringe over a period of 15-20 minutes under argon at room temperature, and the resulting deep red solution is stirred at room temperature for 1 hour. The solvent is removed under reduced pressure (bath temperature should be below 40° C.), and the black residue is dissolved in 200 ml water. (CH3)3O.BF4 (about 15 g) is added portionwise to the solution until it becomes slightly acidic (pH≈5.5). The aqueous layer is extracted three times with 200 ml of ether, and the combined etheral extracts are washed once with 300 ml of saturated brine solution, once with 300 ml of saturated sodium carbonate solution, and three times with 300 ml of saturated brine solution, dried over anhydrous sodium sulfate and filtered. The solvent is removed using a rotary evaporator and the deep red tarry residue is purified by a silica gel column (200 g) using flash chromatography. Elution by approx. 10% ether in n-hexane gives a deep red syrup, which is solidified upon cooling. Recrystallization from pet-ether at -70° C. gives 25.12 g (80.5%) of pentacarbonyl[phenyl(methoxy)carbene]chromium as deep red crystalline.

1. customof 15-20 minutes
2. customat room temperature
3. customThe solvent is removed under reduced pressure (bath temperature should be below 40° C.)
4. dissolutionthe black residue is dissolved in 200 ml water
5. additionBF4 (about 15 g) is added portionwise to the solution until it
6. extractionThe aqueous layer is extracted three times with 200 ml of ether
7. washthe combined etheral extracts are washed once with 300 ml of saturated brine solution, once with 300 ml of saturated sodium carbonate solution, and three times with 300 ml of saturated brine solution
8. dry with materialdried over anhydrous sodium sulfate
9. filtrationfiltered
10. customThe solvent is removed
11. customa rotary evaporator
12. customthe deep red tarry residue is purified by a silica gel column (200 g)
13. washElution by approx. 10% ether in n-hexane
14. customgives a deep red syrup, which
15. temperatureupon cooling
16. customRecrystallization from pet-ether at -70° C.