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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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KBS41-1 - NBS reaction on KBS36 #124

Closed KlementineJBS closed 1 year ago

KlementineJBS commented 1 year ago

Link to HIRAC.

HIRAC NBS reaction Breaking Good.docx

Reaction scheme

KBS41 - NBS reaction on KBS36

Outcome

205.9 mg (of which 195.2 calculated to be product - 61% conversion rate and 72% yield.)

KlementineJBS commented 1 year ago

17.08.23

  1. Dissolved SM (194.7 mg, 0.987 mmol) in MeCN (40 mL)
  2. Added tosic acid (261 mg, 1.52 mmol, 1.5 equiv.) and NBS (217 mg, 1.22 mmol, 1.2 equiv.)
  3. Left stirring at 82 C from 9.15 am
KlementineJBS commented 1 year ago

TLC at 5 pm yesterday (left) and 11 am today (right).

Decided to work up rather than leave over the weekend.

  1. Removed MeCn by rotary evaporation.
  2. Dissolved in DCM (20 mL)
  3. Washed with water (2 x 20 mL) and brine (25 mL)
  4. Dried over mag sulphate and rotovapped down

empty vial: 15.5718 Full vial: 15.7777 Mass: 205.9 mg

KlementineJBS commented 1 year ago

H NMR

Shows approximately 61% conversion for a 72% yield. (SM peak = 2.79, product = 4.88).

KBS41-1 crude_1.zip KBS41-1 cr.pdf