HRID1615323

反应详情

EQUATION

反应方程式

HRID 1615323 的结构方程式

PROCEDURE

实验过程

Synthesized according to the method of Example A19, utilizing indolin-2-one (10.4 mg, 0.0.78 mmol) and (E)-3-(4-((dimethylamino)methyl)styryl)-1-((2-(trimethylsilyl)-ethoxy)methyl)-1H-indazole-6-carbaldehyde (33.4 mg, 0.077 mmol). The crude mixture was concentrated under reduced pressure and purified by prepTLC (SiO2 10% MeOH/DCM) to provide the title compound to as a 1.5-2.0:1.0 (E:Z) mixture of isomers: a yellow solid (29.1 mg, 67%): 1H NMR (400 MHz, CD3OD) δ ppm 9.09-9.14 (s, 0.31H), 8.22 (d, J=8.28 Hz, 0.84H), 8.09 (d, J=8.53 Hz, 0.34H), 7.83-7.87 (m, 1.25H), 7.61-7.69 (m, 4.02H), 7.56-7.60 (m, 1.69H), 7.50 (s, 0.61H), 7.36-7.48 (m, 3.85H), 7.24 (t, J=7.78 Hz, 1.48H), 7.03 (t, J=7.28 Hz, 0.48H), 6.92 (d, J=7.53 Hz, 1.01H), 6.81-6.89 (m, 1.49H), 5.80 (s, 0.60H), 5.78 (s, 1.52H), 3.59-3.65 (m, 2.20H), 2.37-2.42 (m, 7.40H), 0.89 (t, J=8.28 Hz, 3.05H), −0.09 (s, 9H); MS ESI 551.4 [M+H]+, calcd for [C33H38N4O2Si+H]+ 551.8.

WORKUP

后处理

  1. customSynthesized
  2. concentrationThe crude mixture was concentrated under reduced pressure
  3. custompurified by prepTLC (SiO2 10% MeOH/DCM)