HRID1685122

反应详情

EQUATION

反应方程式

HRID 1685122 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

10 mL of methanol was added to a flask containing 16F (0.50 g, 0.85 mmol) prepared in the previous step and 10% Pd/C (0.05 g). The reaction flask was evacuated and purged with hydrogen, then stirred under a balloon of hydrogen overnight at RT. The mixture was filtered over a pad of Celite and the filtrate was concentrated in vacuo. The residue was reconstituted in ethyl acetate, washed with brine, dried over MgSO4, and concentrated to give tert-butyl 4-(2-oxo-5-phenyl-1-(piperidin-3-yl)-2,3-dihydro-1H-imidazole-4-carbonyl)piperazine-1-carboxylate (16H), as a glassy oil in quantitative yield. ESI-MS: m/z 456.4 (M+H)+.

WORKUP

后处理

  1. customThe reaction flask was evacuated
  2. custompurged with hydrogen
  3. filtrationThe mixture was filtered over a pad of Celite
  4. concentrationthe filtrate was concentrated in vacuo
  5. washwashed with brine
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated