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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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KBS19-2 - Deprotection of bis-methylferrocenylcyclam #65

Open KlementineJBS opened 1 year ago

KlementineJBS commented 1 year ago

Link to HIRAC, original method and master page.

KBS19 Deprotection of bis-methylferrocene cyclam.docx

Previous attempt is #21

Reaction scheme

KBS19 Bis-methylferrocene cyclam deprotection

Outcome

Over 100%, needs to be purified. Will use prep HPLC.

KlementineJBS commented 1 year ago

20.03.23

  1. Used 187.9 mg KBS18-2 (0.196 mmol)
  2. Added dioxane (3 mL) and 2 drops water and cooled in ice bath
  3. Added HCl (4 M in dioxane, 1 mL)
  4. Left stirring from 3 pm

Reaction mixture was non homogenous at first (see image). After sonication it was a more uniform mustard yellow.

KlementineJBS commented 1 year ago

Yield

vial before reaction: 15.5851 vial after reaction: 15.7593 mass: 174.2 mg, 0.210 mmol, 107%

KlementineJBS commented 1 month ago

image

KlementineJBS commented 1 month ago

LRMS

F16 - 759.3+ [M+H]+ of product F17 - 973+ [M+Na]+ of SM

KlementineJBS commented 1 month ago

HPLC

image image image image image image

KlementineJBS commented 1 month ago

image image image

KlementineJBS commented 1 month ago

KBS19-2 prep2 F5.pdf KBS19-2 prep2 F5.d.zip

KlementineJBS commented 4 weeks ago

image