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 solution 10-ethoxy-14-methoxy-N-methyl-20-(trifluoromethyl)-9-oxa-4,5,16,18,22,25,28-heptaaza-10-phosphapentacyclo[21.2.2.212,15.12,5.117,21]hentriaconta-1(25),2(31),3,12,14,17(28),18,20,23,26,29-undecaene-24-carboxamide 10-oxide (Example 6, 30.0 mg, 0.0464 mmol) in concentrated HCl (6.0 mL) was stirred at 50° C. for 72 hours. The reaction mixture was concentrated under reduced pressure to a yellow foam. The material was purified on a Teledyne ISCO Combiflash® Rf system using a reverse phase column with Water/MeOH (100:0→0:100) as eluent to afford the title compound as 7.5 mg of a white solid (26%). 1H NMR (400 MHz, CD3OD): δ=8.41 (br. s., 1H), 8.31 (s, 1H), 8.27 (br. s., 1H), 7.87 (d, J=6.6 Hz, 1H), 7.59 (d, J=6.6 Hz, 1H), 7.45 (d, J=6.6 Hz, 1H), 6.70 (br. s., 1H), 6.27 (d, J=4.8 Hz, 1H), 4.42 (br. s., 2H), 3.83 (br. s., 3H), 3.52 (br. s., 2H), 2.93 (s, 3H), 2.80 (d, J=17.4 Hz, 2H), 2.16 (br. s., 2H). MS (ESI): m/z 619.17 [M+H]+. UPLC: tR=0.80 min (polar—2 min).
WORKUP
后处理
- concentrationThe reaction mixture was concentrated under reduced pressure to a yellow foam
- customThe material was purified on a Teledyne ISCO Combiflash® Rf system