Ammonia → HCID 69516679, compound

Participants

Reaction Steps

415 mg (1.30 mmol) of TBTU are added to a suspension (500 mg, 1.30 mmol) of the compound obtained in Step B of Example 2 in 25 ml of CH2Cl2. The suspension is stirred at ambient temperature for 10 minutes and 293 μl (1.68 mmol) of diisopropylethylamine are added. The reaction mixture becomes a solution and stirring is continued for 10 minutes. The solution is then saturated with ammonia gas and stirring is continued for 30 minutes. Thin-layer chromatography (AcOEt) indicates that all the starting material has disappeared. The reaction mixture is then acidified by adding 1N HCl; the organic phase is decanted off, washed (water and then saturated NaCl solution), dried (MgSO4) and evaporated. The residue is triturated in Et2O and the white solid formed is filtered off to yield the title product.

Provenance & Evidence