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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_8B_1 - Hydrolysis on 2-amino-methoxypyridine fragment #87

Closed KlementineJBS closed 1 year ago

KlementineJBS commented 1 year ago

Reaction scheme

2023_BG_8B

Outcome

390.3 mg (2.13 mmol, 76%)

KlementineJBS commented 1 year ago
  1. Dissolved SM (804 mg, 2.80 mmol) in NaOH (2.5 M, 5 mL)
  2. Stirred at 80 C for 45 minutes

TLC indicated completion.

Work up as usual - see step 2.

KlementineJBS commented 1 year ago

LRMS

Peaks at 184.13 [M+H]+ and 206.11 [M+Na]+ confirm product is present,

2023_BG_8B_1.d.zip 2023_BG_8B_1.pdf

KlementineJBS commented 1 year ago

Vial empty: 15.3002 Vial full: 15.6905 Mass: 390.3 mg (2.13 mmol, 76%)

KlementineJBS commented 1 year ago

NMR

1H NMR (500 MHz, DMSO-d6) δ 10.41 (s, 1H), 10.33 – 10.29 (m, 1H), 8.68 (s, 1H), 7.95 (d, J = 3.0 Hz, 1H), 7.46 (dd, J = 9.1, 3.1 Hz, 1H), 7.16 (d, J = 9.1 Hz, 1H), 3.79 (s, 3H).

13C NMR (126 MHz, DMSO) δ 180.33, 151.62, 148.11, 131.61, 126.35, 114.07, 56.35.

2023_BG_8B 500 MHz.pdf 230709_8B_1.zip 230709_8B_2.zip