HRID1922435

反应详情

EQUATION

反应方程式

HRID 1922435 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2-(8-Fluoro-6-nitro-3,4-dihydroquinolin-1(2H)-yl)-N,N-dimethylethanamine (340 mg, 1.27 mmol) was weighed into a round bottom flask equipped with a stir bar. Ethanol (8 mL) was 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 reaction mixture was stirred for 2 h at room temperature under balloon pressure. The reaction mixture was then filtered through a pad of celite and the pad washed with methanol. The filtrate was concentrated, then chromatographed on silica gel using 0-10% (2M NH3 in MeOH) in dichloromethane. Yield: 270 mg, 89%. ESI-MS: 238 (MH+, 100), 193 (37), 147 (31).

WORKUP

后处理

  1. customequipped with a stir bar
  2. customevacuated of air
  3. filtrationThe reaction mixture was then filtered through a pad of celite
  4. washthe pad washed with methanol
  5. concentrationThe filtrate was concentrated
  6. customchromatographed on silica gel using 0-10% (2M NH3 in MeOH) in dichloromethane