反应详情

温度

-78 °C

A 300 ml stainless steel autoclave was charged with 2.00 g manganese (II) acetate (11.6 mmol), 3.07 g cyclopentadiene monomer (46.5 mmol), 70 ml ether, and 4.0 g TEA (35.1 mmol) pre-mixed with some of the ether. The autoclave was sealed and purged with CO. The carbonylation was carried out at 550 psi total pressure and a temperature of 175° C. for two hours. The cooled reactor was vented and the contents transferred to an Erlenmeyer flask. A solution of 10% HCl was added carefully until the salts dissolved. The organic layer was separated and washed with water, dried (MgSO4), filtered and evaporated leaving a red oil. Pentane (100 ml) was added. Cooling to -78° C. for several hours gave 1.10 g (54%) of cyclopentadienylmanganese tricarbonyl product as yellow crystals, mp 65°-69° C.

1. customThe autoclave was sealed
2. custompurged with CO
3. additionA solution of 10% HCl was added carefully until the salts
4. dissolutiondissolved
5. customThe organic layer was separated
6. washwashed with water
7. dry with materialdried (MgSO4)
8. filtrationfiltered
9. customevaporated
10. customleaving a red oil