HRID1922432

反应详情

EQUATION

反应方程式

HRID 1922432 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

1-(2-(Dimethylamino)ethyl)-8-fluoro-6-nitro-3,4-dihydroquinolin-2(1H)-one (500 mg, 1.77 mmol) was weighed into a round bottom flask equipped with a stirbar. Ethanol (10 mL) and THF (2 mL) were added, followed by Pd, 10 wt. % on activated carbon. The flask was fitted with a balloon of hydrogen, evacuated of air and backfilled with hydrogen. The black suspension was stirred for 3 h at room temperature. The solid palladium was then filtered off through a plug of celite and the celite pad washed with methanol. The filtrate was concentrated, then chromatographed on silica gel using 0-10% (2M NH3 in MeOH) in ethyl acetate to give the product. Yield: 325 mg, 72%. EI-MS: 251 (M+, 3), 58 (100).

WORKUP

后处理

  1. customequipped with a stirbar
  2. customevacuated of air
  3. filtrationThe solid palladium was then filtered off through a plug of celite
  4. washthe celite pad washed with methanol
  5. concentrationThe filtrate was concentrated
  6. customchromatographed on silica gel using 0-10% (2M NH3 in MeOH) in ethyl acetate
  7. customto give the product