HRID77439

反应详情

EQUATION

反应方程式

HRID 77439 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 8-fluoro-2-oxo-1,2,3,4-tetrahydroquinolin-6-yl acetate (1.3 g, 5.82 mmol) in MeOH (50 mL) at room temperature was added 1N NaOH (11.65 mL, 11.65 mmol). The reaction mixture was stirred at room temperature overnight, then concentrated to a yellow oil. This was diluted with water and acidified with conc. HCl to pH 1. The precipitate was collected by filtration, washed with water, and recrystallized from MeOH/water to give 8-fluoro-6-hydroxy-3,4-dihydroquinolin-2(1H)-one as a white solid (0.46 g, 44%). 1H NMR (400 MHz, METHANOL-d4) δ ppm 6.57-6.48 (m, 2H), 2.93 (s, 2H), 2.56 (dd, J=7.9, 6.9 Hz, 2H). LCMS: R.T.=1.125 min; [M+H]+=182.1.

WORKUP

后处理

  1. concentrationconcentrated to a yellow oil
  2. additionThis was diluted with water
  3. filtrationThe precipitate was collected by filtration
  4. washwashed with water
  5. customrecrystallized from MeOH/water