1,2-Dichloroethane → HCID 24753121, compound

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Reaction Steps

The compound from Step A above was dissolved in 0.5 mL each of THF, methanol and water then 12.0 mg (0.5 mmol) of lithium hydroxide was added and the solution was stirred for 18 h at rt. The solution was allowed to cool to room temperature and 300 μL of 2 N HCl was added. The solvent was evaporated and the residue was dissolved in 500 μL of DMF. Phenylenediamine (104 mg, 0.500 mmol), EDC (96.7 mg, 0.500 mmol), and HOBt (67.2 mg, 0.500 mmol) were added and the solution was allowed to stir for 18 h. The solution was diluted with 50 mL of CH2Cl2 and washed with 50 mL each of NaHCO3 and brine. The solution was concentrated and purified by reverse phase HPLC to give the desired product. MS cal'd 495 (MH+), exp 495 (MH+).

Provenance & Evidence