HRID1772601
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 of compound 6b (220 mg, 0.470 mmol) and CDI (200 mg, 1.23 mmol) in THF (8 mL) was stirred at rt for 18 h. The reaction was quenched with H2O (10 mL). The resulting solids were collected by filtration and washed with Et2O to obtain the title compound 94 as a light yellow solid (57.6 mg, 25% yield). 1H-NMR (300 MHz, DMSO-d6) δ (ppm): 11.62 (s, 1H), 11.08 (s, 1H), 8.33 (d, J=8.4 Hz, 1H), 8.21 (s, 1H), 8.11 (s, 1H), 7.97-7.92 (m, 2H), 7.86-7.80 (m, 2H), 7.74 (t, J=7.8 Hz, 1H), 7.66 (s, 1H), 7.60-7.51 (m, 2H), 7.39 (s, 1H), 4.40-4.25 (m, 4H), 3.95-3.75 (m, 4H). Mass Spectrum (LCMS, ESI pos.): Calcd. for C27H22N8O2: 491.2 (M+H). Found 491.0.
WORKUP
后处理
- customThe reaction was quenched with H2O (10 mL)
- filtrationThe resulting solids were collected by filtration
- washwashed with Et2O