反应详情

tert-Butyl 3-[9-[1-(4-amino-3-methyl-1H-pyrazolo[3,4-d]pyrimidin-1-yl)ethyl]-7-chloro-6-methyl-2,3-dihydro-1,4-benzoxazepin-4(5H)-yl]azetidine-1-carboxylate (15 mg, 0.035 mmol) was treated with 4 N HCl in dioxane (1 mL), and then the solvent was evaporated. The residue was stirred in N,N-dimethylformamide (0.5 mL) with N,N-diisopropylethylamine (10 μL, 0.06 mmol) and acetic anhydride (20 μL, 0.2 mmol) was added. The mixture was stirred for 5 minutes and diluted with methanol. Purification by preparative LCMS (pH 10) gave the desired compound (2.2 mg, 13%). LCMS calculated for C23H29ClN7O2 (M+H)+: m/z=470.2; found: 470.2. 1H NMR (300 MHz, CD3OD): δ 8.14 (s, 1 H), 7.33 (s, 1 H), 6.33 (m, 1 H), 4.27 (m, 1 H), 4.02 (m, 2 H), 3.80 (m, 1 H), 3.72 (m, 1 H), 3.69 (m, 3 H), 3.48 (m, 1 H), 2.79 (m, 2 H), 2.58 (s, 3 H), 2.38 (s, 3 H), 1.82 (m, 3 H), 1.77 (m, 3 H).

1. customthe solvent was evaporated
2. additionwas added
3. customPurification by preparative LCMS (pH 10)