Ferrocene_procedures

Ferrocene_procedures - ExFrimental Procedurc 2.5rnl...

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ExFrimental Procedurc Using a microscale simple distillation setup, heated 2.5rnl mineral oil to 250"c. Dicyclopentadiene (0.989, 7.4lmrnol) added drcpwise over lO minutes. Collected and cooled cyclopentadiene product. Pota$sium hydrcxid€ (0.759) and DME (l.25ml) combin€d and degassed with nitrogen for I minute. Injected degass€d mixtue with 0.30OmL of cooled cycloFntadiene product and vigorously stined mixtur€ until color changcd from white to led. Gr€en R(II) chloride tetrahydrate (0.359) and DMSo (l.5mL) combined and degassed with nitrogen for I minute in separate flask. Added contents to first mixturE over 15 minutes, rinsed second flask with additional DMSO (O.25ml) and added lo mixturE. Stifled dark s]urry with HCI acid (4.5mL' 6M) and 59 ice' in a clean beaker, until dissolved. Orange crystals were collected and washed then dried using a HiNch funnel. Sublimcd crude product (orange crystals) orto a centrifuge tube (l5mm) filled with icc, which ielded the pule product
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This note was uploaded on 09/09/2008 for the course CHEM 245 taught by Professor Burdette during the Spring '08 term at UConn.

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Ferrocene_procedures - ExFrimental Procedurc 2.5rnl...

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