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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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KBS32-1 - Hydrolysis on 2-amino-5-methylpyridine fragment #110

Closed KlementineJBS closed 11 months ago

KlementineJBS commented 1 year ago

Reaction scheme

KBS31 and KBS32

Outcome

462 mg, 88%

KlementineJBS commented 1 year ago
  1. Dissolved 853 mg (3.14 mmol) KBS31-1 (#109) in NaOH (2.5 M, 2.5 mL)
  2. Added 1 mL water (to wash down SM stuck to funnel)
  3. Heated to 80 C with stirring for 2 hours
  4. Cooled on ice
  5. Adjusted to pH 10-11
  6. Vacuum filtered and collected fine powdery white precipitate

Empty vial: 15.7181 Full vial: 16.1800 Mass: 461.9 mg (2.76 mmol, 88%)

KlementineJBS commented 1 year ago

NMR

1H NMR (300 MHz, DMSO-d6) δ 10.55 – 10.48 (m, 1H), 10.44 (s, 1H), 8.78 (s, 1H), 8.07 (d, J = 2.3 Hz, 1H), 7.61 (dd, J = 8.4, 2.4 Hz, 1H), 7.09 (d, J = 8.4 Hz, 1H), 2.23 (s, 3H).

KBS32-1_1.zip KBS32-1.pdf

KlementineJBS commented 1 year ago

LRMS

Peaks at 190.10 [M+Na]+, 357.04 [2M + Na]+, 166.03 [M-H]- confirm presence of product.

KBS32-1.pdf KBS32-1.d.zip