Hydrazine hydrate (1:1) → 2-Benzyloxy-N4-(4,6-bis-((3R,5S)-3,5-bis-(tert-butoxycarbonylamino)-piperidin-1-yl)-[1,3,5]triazin-2-yl)-benzene-1,4-diamine

関与物質

反応手順

N-[2-Benzyloxy-4-(4,6-bis-((3R,5S)-3,5-bis-(tert-butoxycarbonylamino)-piperidin-1-yl)-[1,3,5]triazin-2-ylamino)-phenyl]-acetamide (401) (2.32 g, 2.4 mmol) was dissolved in an mixture of MeOH and dioxane (150 mL, 4:1). Hydrazine monohydrate (100 mL) was added and the mixture was heated to reflux for 10 days. LC-MS indicated complete de-protection at this point. Upon cooling, a white precipitate formed. The mixture was poured into ice water, forcing additional precipitate to form. The solid was collected by filtration under reduced pressure, rinsed with water (100 mL), and dried under high vacuum for 16 h to give the desired product (402) as a white powder (1.48 g, 1.62 mmol, 68% yield). LC-MS (ESI): (exact mass: 919.53) m/e=920.6 [M+1]+ (100%).

情報源と証拠