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
CONDITIONS
反应条件
- 温度
- 90 °C
PROCEDURE
实验过程
To a suspension of 8-indan-5-yl-2-methanesulfonyl-5-oxo-5,8-dihydro-pyrido[2,3-d]pyrimidine-6-carboxylic acid amide (from Example 23 (b), 7 mg) in 1 mL of i-PrOH was added 3-(4-methyl-piperazin-1-ylmethyl)-phenylamine (5 mg). The mixture was stirred at 90° C. for 1 hr. After cooling down, the solvent was evaporated and the product was purified chromatographically (CH2Cl2/CH3OH/NH4OH (10:1:0.1, v/v)). The title compound was obtained as white solid (2.7 mg, 29%). 1H NMR (400 MHz, CDCl3) δ (ppm): 9.39 (br, 1H), 9.34 (s, 1H), 8.76 (s, 1H), 7.48 (br, 1H), 7.35 (d, J=8.0 Hz, 1H), 7.29 (br, 1H), 7.17 (s, 1H), 7.12 (d, J=8.0 Hz, 1H), 6.94 (br, 2H), 5.67 (br, 1H), 3.29 (br, 2H), 3.00 (t, J=7.3 Hz, 2H), 2.92 (t, J=7.3 Hz, 2H), 2.49 (br, 7H), 2.33 (br, 4H), 2.15 (m, 2H). Mass Spectrum (LCMS, ESI pos.) Calcd. For C29H31N7O2: 510.25 (M+H), Found: 510.1.
WORKUP
后处理
- temperatureAfter cooling down
- customthe solvent was evaporated
- customthe product was purified chromatographically (CH2Cl2/CH3OH/NH4OH (10:1:0.1