HRID1772594
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
Compound 2c (120 mg, 0.260 mmol) was treated with NaN3 as described in Example 1, Step H. This resulted in 150 mg of crude compound 96, which was then purified by Prep-HPLC under the following conditions: XbridgePrep Shield RP 18, 5 μm, 19*150 mm; mobile phase, water with 0.05% NH4CO3 and CH3CN (30% CH3CN up to 50% in 8 min, up to 100% in 1 min, down to 30% in 1 min); Detector, UV 254 nm. The title compound 96 was obtained as a yellow solid (38.4 mg, 29% yield). 1H-NMR (300 MHz, DMSO-d6) δ (ppm): 9.09 (s, 1H), 8.41-8.33 (m, 4H), 7.95-7.56 (m, 8H), 4.50-4.28 (m, 4H), 4.00-3.71 (m, 4H). Mass Spectrum (LCMS, ESI pos.): Calcd. for C22H22N10O: 503.2 (M+H). Found 503.2.
WORKUP
后处理
- customThis resulted in 150 mg of crude compound 96, which
- customwas then purified by Prep-HPLC under the following conditions
- waitup to 100% in 1 min
- waitdown to 30% in 1 min)