Phosphonium Coupling Reagent Kit 2
HCK1005-01-006

2 sets of 7 reagents; PyBOP®, PyAOP, TPTDP, BroP, PyBroP, DEPBT, and ethyl(hydroxyimino)cyanoacetate
This kit requires EvoluChem reaction block (HCK1006-01-002) included in the EvoluChem Starter Kit (HCK1006-01-001)

The typical protocol is performed at 0.1 mol/l concentration reaction condition using a solution of combined acid and amine. However you can a different ratio of amine and acid. Recommended solvents are CH2Cl2, DMF or NMP. Solvent should be selected based on solubility of the substrates. Recommended bases are Et3N or DIPEA.

Protocol at 100 µl volume reaction condition

  1. Prepare required volume of a solution of combined amine 0.1 mol/L and acid substrate 0.1 mol/L in the desired solvent. For example, 700 µl solution for 6 reaction conditions (100 µl extra to compensate potential evaporation).
  2. Add 2 equivalents of base (Et3N or DIPEA) to the solution see table
  3. Using a clean and dry syringe, add 100 µl of solution to each reaction vial containing coupling reagent.
  4. Optional: Add 10 µl of the solution of ethyl (hydroxyimino) cyanoacetate to each reaction vial. (prepared by adding 70 µl of DMF in the reagent vial)
  5. Stir the reaction vials in the reaction block at desired temperature for 3 to 12 hours. Do not heat vials at temperature higher than 120°C or higher than 5°C above the boiling point of the used solvent.
  6. Remove the vial caps using a decapper.
  7. Prepare analytical sample for each reaction condition with 5 µl sample diluted into 200 µl in either DMSO or water/acetonitrile 50/50. Analyze resulting analytical samples by LC/MS.

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