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KlementineJBS / USYD_PhD_ELN

This repository forms the electronic laboratory notebook (ELN)for Klementine Burrell-Sander's PhD's
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KBS29-5 - Bromination of KBS28 with phosphorus tribromide #154

Closed KlementineJBS closed 7 months ago

KlementineJBS commented 8 months ago

Link to HIRAC and master page #164 . Method taken from J. Batten's PhD thesis (2022).

KBS29 - Appel reaction (CBr4).docx

Previous attempt is #148

Reaction scheme

KBS29 - Phosporus tribromide reaction

Outcome

159.6 mg, 0.554 mol, 62%

KlementineJBS commented 8 months ago

06.11.23

SM = 202 mg, 0.897 mmol Added PBr3 (288 mg, 1.076 mmol, 101 uL).

Put reaction on at about 3.30 pm. Initially was a clear straw yellow, but had turned cloudy after an hour or so.

initially

After 1.5 hrs

TLC confirmed completion at 5 pm. A faint second product had appeared close to the baseline.

Quenched with NaHCO3 (10 mL), then worked up with DCM (3 x 10 mL) and washed with NaHCO3 (10 mL) before drying over mag sulphate and rotovapping. Some product lost to spill.

Empty vial: 15.6849 Full vial: 15.8445 Mass: 159.6 mg, 0.554 mol, 62%

KlementineJBS commented 7 months ago

H NMR

Mostly clean, with some solvent impurities. Can probably carry through as is.

KBS29-5 cr_1.zip KBS29-5 cr.pdf

KlementineJBS commented 7 months ago

Column conditions

image