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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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2023_BG_9B_2 - Hydrolysis on 2-amino-6-fluoropyridine fragment #97

Closed KlementineJBS closed 1 year ago

KlementineJBS commented 1 year ago

Reaction scheme

2023_BG_9B

Outcome

6.129 g (35.8 mmol, 82%)

KlementineJBS commented 1 year ago
  1. Dissolved SM (11.9699 g (43.5 mmol) in NaOH (2.5 M, 35 mL)
  2. Heated to 80 C from 9.10 am to 10.50 am.

TLC indicated completion.

Work up as usual - see step 2.

KlementineJBS commented 1 year ago

Vial 1: 15.6547 Full vial: 19.1298 Mass: 3.4751 g

Vial 2: 15.6820 Full vial: 18.3359 Mass: 2.6539 g

Total mass = 6.129 g (35.8 mmol, 82%)

KlementineJBS commented 1 year ago

LRMS

Peak at 170.03 [M-H]-. Unsure whether peak at 136.10 (-1) is from sample or contaminant. Has shown up in a few hydrolysis products.

2023_BG_9B_2.pdf 2023_BG_9B_2.d.zip

KlementineJBS commented 1 year ago

H NMR

Matches with spectrum from #86

2023_BG_9B_2_1.zip 2023_BG_9B_2.pdf

KlementineJBS commented 1 year ago

Recrystallisation

Recrystallised using methanol.

NMR

2023_BG_9B_2 crystals.pdf 2023_BG_9B_2 crystals_1 (1).zip