تفاعل #73111
ord-be3c8205d6884974975dca17f1976345
معادلة التفاعل
الكواشف
لا شيء
المذيبات
ظروف التفاعل
درجة الحرارة
100°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1تركيزThe solution was concentrated under vacuum
- 2أخرىthe crude material was purified by preparative HPLC
الإجراء التجريبي
The title compound was prepared by dissolving (R)-methyl 1-(8-cyclopentyl-7-ethyl-5-methyl-6-oxo-5,6,7,8-tetrahydropteridin-2-yl)-1H-imidazole-4-carboxylate (Example 38, 0.51 g, 1.33 mmol) in 2 mL of acetic acid and 0.5 mL of concentrated aqueous HCl and heating the resulting solution to 100° C. for 4 hours. The solution was concentrated under vacuum and co-evaporated from toluene three times and the crude material was purified by preparative HPLC. 1H NMR (CDCl3) δ: 8.73 (s, 1H), 8.50 (s, 1H), 7.78 (s, 1H), 4.44-4.45 (m, 1H), 4.32-4.36 (m, 1H), 3.39 (s, 3H), 1.71-2.17 (m, 10H), and 0.92 ppm (t, J=7.6 Hz, 3H); LCMS: 371.1 m/z (M+H)+; ret. Time: 3.008 min (Analytical Method A).