KlementineJBS / USYD_PhD_ELN

This repository forms the electronic laboratory notebook (ELN)for Klementine Burrell-Sander's PhD's

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Closed KlementineJBS closed 6 months ago

KlementineJBS commented 6 months ago

Link to HIRAC.

Reaction scheme

KBS29 - Phosporus tribromide reaction

KlementineJBS commented 6 months ago

Identifier	Link	Yield (%)	Further info
1	#57	75	1.7 equiv. of CBr4 and PPh3, stirred for 2 days - possibly worked up with SM still present
2	#63	-	hard to purify/quantify. Left over a week and used KBr. 2.2 equiv. of CBr4 and PPh3, 0.5 equiv. of KBr. worked up with SM still present.
3	#148	53	PBr3, 3 hours
4	#152	-	CBr4, abandoned due to contamination
5	#154	62	PBr3
6	#156	35	PBr3
7	#162	23%, some unpurified material remaining	PBr3

KlementineJBS commented 6 months ago

Methylene peak shifts from 4.98 to 4.74, giving strong evidence that Br product has formed.

KlementineJBS commented 6 months ago

Make sure to do PBr3 reaction under nitrogen and use ice bath/dropwise addition of PBr3 to account for exothermic effect at scale.

KlementineJBS commented 5 months ago

Mesylate KBS28 before attempting bromination. E.g. using protocol from this paper

KlementineJBS commented 4 days ago