Ammonia → HCID 59349647, compound

Participants

Reaction Steps

155 mg (0.395 mmol) of the compound from Example 31A are introduced into 10 ml of THF and, after addition of 80.1 mg (0.494 mmol) of 1,1′-carbonyldiimidazole, stirred at room temperature overnight. A TLC check (silica gel; mobile phase: ethyl acetate or dichloromethane/methanol 9:1) shows complete conversion. The volatile components are removed in a rotary evaporator, and the residue is taken up in 3 ml of DMF. Then 553 mg of ammonia (28% by weight solution in water, 3.95 mmol) are added, and the reaction mixture is heated at 100° C. for 10 min. The solvent is removed under reduced pressure, and the residue is purified by preparative HPLC (eluent: acetonitrile/water with 0.1% formic acid, gradient 20:80→95:5). 30 mg (19% of theory) of the title compound are obtained.

Provenance & Evidence