反应详情

7-chloro-3-(4-methoxybenzyl)-1-trityl-1,3,4,5-tetrahydropyrazolo[3,4,5-de][1,6]naphthyridine (40 mg, 0.072 mmol), (S)-1-(2-hydroxy-2-methyl-1-phenylpropyl)urea (22.4 mg, 0.108 mmol), cesium carbonate (82 mg, 0.25 mmol) and BrettPhos pre-catalyst (6.5 mg, 7.18 μM) were charged in a 1 dram vial, evacuated and backfilled with nitrogen and taken in 1,4-dioxane (0.4 mL) and heated reaction to 100° C. for 30 minutes. The reaction mixture was diluted with DCM, washed with water, brine, dried with sodium sulfate and concentrated. Purification of the residue by flash column (0-75% EtOAc-hexanes) gave (S)-1-(2-hydroxy-2-methyl-1-phenylpropyl)-3-(3-(4-methoxybenzyl)-1-trityl-1,3,4,5-tetrahydropyrazolo[3,4,5-de][1,6]naphthyridin-7-yl)urea. MS ESI calc'd. for C46H44N6O3 [M+H]+ 729. found 729.

1. customevacuated
2. temperatureheated
3. customreaction to 100° C. for 30 minutes
4. washwashed with water, brine
5. dry with materialdried with sodium sulfate
6. concentrationconcentrated
7. customPurification of the residue by flash column (0-75% EtOAc-hexanes)