反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A suspension of tert-butyl 2-(4-((5-fluoropyridin-2-yl)methoxy)-2-oxopyridin-1(2H)-yl)-10-methyl-7,8,9,10-tetrahydropyrido[3′,2′:4,5]pyrrolo[3,2-c]azepine-6(5H)-carboxylate (130 mg, 0.250 mmol) in 1.25 M HCl in MeOH (4.0 mL) was stirred at ambient temperature for 72 h. The solution was concentrated and dried to provide the title compound (108 mg, 95%) as a brown-yellow powder: 1H NMR (500 MHz, DMSO-d6) δ 9.15 (s, 2H), 8.62 (d, J=3.0 Hz, 1H), 8.16 (d, J=8.5 Hz, 1H), 7.88-7.80 (m, 2H), 7.67-7.64 (m, 1H), 7.35 (d, J=8.0 Hz, 1H), 6.19 (dd, J=8.0, 2.5 Hz, 1H), 5.99 (d, J=2.5 Hz, 1H), 5.23 (s, 2H), 4.46 (s, 2H), 3.75 (s, 3H), 3.49-3.40 (m, 2H), 3.36-3.20 (m, 2H), 2.19-2.08 (m, 2H); ESI MS m/z 420 [M+H]+; HPLC (Method A) 98.2% (AUC), tR=12.2 min.
WORKUP
后处理
- concentrationThe solution was concentrated
- customdried