HRID2175360

反应详情

EQUATION

反应方程式

HRID 2175360 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 2-[-2-(5,8-Dimethyl-[1,2,4]triazolo[1,5-a]pyrazin-2-yl)-vinyl]-5H-imidazo[2,1-a]isoindole (139 mg, 0.423 mmol) in methanol (100 mL) was added 10% palladium on carbon (27 mg). A current of hydrogen gas was bubbled through, and the reaction was kept under an atmosphere of hydrogen overnight with stirring. After filtration the organics were evaporated onto silica gel (2 g). Chromatography (gradient elution, A:B 100:0 to 0:100, where A is ethyl acetate and B is 10% MeOH in ethyl acetate) afforded the title compound as a white solid (50.6 mg, 36%). 1H NMR (500 MHz, CDCl3): δ 7.86-7.82; (m, 2H), 7.46-7.42; (m, 2H), 7.33; (t, J=7.5 Hz, 1H), 7.02; (s, 1H), 4.84; (s, 2H), 3.44; (dd, j=8.9, 6.6 Hz, 2H), 3.33; (dd, J=8.9, 6.6 Hz, 2H), 2.91; (s, 3H), 2.73; (s, 3H) LC-MS: m/z=331.0 (MH+), tR=0.74 minutes.

WORKUP

后处理

  1. customA current of hydrogen gas was bubbled through, and the reaction
  2. filtrationAfter filtration the
  3. customorganics were evaporated onto silica gel (2 g)
  4. washChromatography (gradient elution