1,2-Dimethoxyethane → Bis(eta-cyclopentadienyl) iron

In a dry 2-L flask equipped with a mechanical stirrer and a reflux condenser topped with a nitrogen-inlet tube was charged with 1L of DME and 193 g (1.6 mol) of KOtBu. Under N2 atmosphere, 8.8 mL (0.48 mol) of water was added to the crude (2-chlorobenzoyl) ferrocene to give a red solution. The red solution was stirred and refluxed under N2. As the reaction proceeded with fade of color to tan. The reaction mixture was cooled and poured into 2 L of water. The resulting solution was washed with 2×400 mL of Et2O. The combine organic layer was extracted with 2×200 ml of 10% NaOH. The aqueous phase are then combined and acidified with concentrated HCl. The precipitate was collected by filtration and was dried in are to give yellow power 1 (76 g, 82.6%).

1. customtopped with a nitrogen-inlet tube
2. customto give a red solution
3. temperaturerefluxed under N2
4. temperatureThe reaction mixture was cooled
5. washThe resulting solution was washed with 2×400 mL of Et2O
6. extractionThe combine organic layer was extracted with 2×200 ml of 10% NaOH
7. filtrationThe precipitate was collected by filtration
8. customwas dried

ORD record

ord-b549f338c70c45edb343fc2d6dfc0b23

Source dataset

uspto-grants-2003_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06534657B2