反应详情

A mixture of 5-chloro-N-[2-methoxy-4-(5-methyl-2,5-diazaspiro[3.4]octan-2-yl)-5-nitrophenyl]-4-pyrazolo[1,5-a]pyridin-3-ylpyrimidin-2-amine (Intermediate 46, 95 mg, 0.18 mmol), iron (61 mg, 1.09 mmol) and NH4Cl (7.32 mg, 0.14 mmol) was heated at reflux in ethanol (10.5 mL) and water (3.5 mL) for 2 h. The mixture was cooled and filtered through diatomaceous earth (Celite™). The filtrate was concentrated in vacuo and the residue was dissolved in CH2Cl2. This solution was washed with brine, dried (Na2SO4) and concentrated in vacuo. Purification by FCC, eluting with 2-6% 7N methanolic ammonia in CH2Cl2 gave the title compound (30 mg, 34%) as a brown gum; m/z: ES+ MH+ 491.5.

1. temperaturewas heated
2. temperatureThe mixture was cooled
3. filtrationfiltered through diatomaceous earth (Celite™)
4. concentrationThe filtrate was concentrated in vacuo
5. dissolutionthe residue was dissolved in CH2Cl2
6. washThis solution was washed with brine
7. dry with materialdried (Na2SO4)
8. concentrationconcentrated in vacuo
9. customPurification by FCC
10. washeluting with 2-6% 7N methanolic ammonia in CH2Cl2