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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_1B_2 - Hydrolysis on 2-fluoroaniline fragment #73

Closed KlementineJBS closed 11 months ago

KlementineJBS commented 1 year ago

Reaction scheme

2023_BG_1B

Outcome

5.39 g (31.7 mmol), 73%

KlementineJBS commented 1 year ago

12.05.23

  1. Dissolved 11.896 g (43..4 mmol) in NaOH (2.5 M, 100 mL)
  2. Heated to 80 C with stirring for ~ 40 minutes

30% ethyl acetate in hexanes, UV

TLC indicated completion.

  1. Cooled to rt
  2. Adjusted to ~ pH 9 with HCl (1 M) and Na2CO3 to form a white precipitate
  3. Cooled on ice to encourage precipitate to form
  4. Vacuum filtered and washed with cold water
  5. Dried under vacuum over the weekend

Beaker: 50.0536 Full beaker: 55.4416 Mass: 5.388 g

KlementineJBS commented 1 year ago

H NMR

2023_BG_1B_2_1.zip 2023_BG_1B_2.pdf

Agrees well with #69 - peaks attributed to amines have shifted slightly but this is to be expected from labile protons.

KlementineJBS commented 1 year ago

LRMS

Peaks at 169.02 [M-H]- and 193.08 [M+H]+.

2023_BG_1B_2.pdf 2023_BG_1B_2.d.zip

MJE thiourea.d.zip MJE thiourea.pdf