反应详情

0.756 g (1.38 mmol) of 1-[p-(1,2,4-triazol-4-yl)phenyl]-4(S)-hydroxy-2-(tert-butyloxycarbonyl)amino-5(S)-(trifluoroacetyl)amino-6-phenyl-2-azahexane (Example 14d) is initially introduced in 28 ml of methanol, and 6.9 ml (6.89 mmol) of a 1 M aqueous solution of potassium carbonate are then added. The reaction mixture is stirred under reflux for 3 h and then concentrated down to about 10 ml; it is then acidified with dilute hydrochloric acid and extracted with methylene chloride. The title compound crystallizes out on concentrating. HPLC20-100: tret=8.97. 1H NMR (CD3OD; 200 MHz) i.a.: 8.98/s (2H); 7.75-7.6/m (4H); 7.5-7.1/m (5H); 3.96/bs (2H); 1.32/s (9H).

1. temperatureunder reflux for 3 h
2. concentrationconcentrated down to about 10 ml
3. extractionextracted with methylene chloride
4. customThe title compound crystallizes out
5. concentrationon concentrating