反应详情

640 mg (1.69 mmol) of the compound from Example 27A are introduced into 30 ml of ethyl acetate and, after addition of 342 mg (2.11 mmol) of 1,1′-carbonyldiimidazole, stirred at room temperature overnight. A TLC check (silica gel; mobile phase: cyclohexane/ethyl acetate 1:1 or dichloromethane/methanol 9:1) shows complete conversion. The volatile components are removed in a rotary evaporator, and the residue is taken up in 20 ml of DMF. Then 2.36 ml of ammonia (28% by weight solution in water, 16.87 mmol) are added, and the reaction mixture is heated at 50° C. for 8 h. The solvent is distilled out under reduced pressure, and the residue is purified by preparative HPLC (eluent: acetonitrile/water with 0.1% formic acid, gradient 20:80→95:5). 368 mg (58% of theory) of the title compound are obtained.

1. customThe volatile components are removed in a rotary evaporator
2. temperaturethe reaction mixture is heated at 50° C. for 8 h
3. distillationThe solvent is distilled out under reduced pressure
4. customthe residue is purified by preparative HPLC (eluent: acetonitrile/water with 0.1% formic acid, gradient 20:80→95:5)