HRID707442

反应详情

EQUATION

反应方程式

HRID 707442 的结构方程式

PROCEDURE

实验过程

To a round bottomed flask was added tert-butyl(trans-4-(3-cyclopropyl-2-oxo-2,3-dihydro-1H-imidazo[4,5-b]pyrazin-1-yl)cyclohexyl)carbamate (0.7301 g, 1.955 mmol, Step 3) and hydrogen chloride, 4.0M solution in 1,4-dioxane (4.89 ml, 19.55 mmol, Sigma-Aldrich Chemical Company, Inc.) to stir at room temperature for 7 h. Precipitate was noted to form. The reaction mixture was filtered and the solid was washed with diethyl ether to give the title compound (209.9 mg, 0.678 mmol, 34.7% yield). 1H NMR (400 MHz, DMSO-d6) δ ppm 0.95-1.10 (m, 4 H) 1.47-1.62 (m, 2 H) 1.85 (d, J=11.15 Hz, 2 H) 2.10 (d, J=11.35 Hz, 2 H) 2.26-2.41 (m, 2 H) 2.93-3.02 (m, 1 H) 3.11 (t, J=11.93 Hz, 1 H) 4.22 (ddd, J=12.23, 8.51, 3.72 Hz, 1 H) 7.91-7.95 (m, 1 H) 7.95-7.99 (m, 1 H) 8.12 (br. s., 2 H)

WORKUP

后处理

  1. customto form
  2. filtrationThe reaction mixture was filtered
  3. washthe solid was washed with diethyl ether