HRID2240188

反应详情

EQUATION

反应方程式

HRID 2240188 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 11-(3-fluorophenyl)-9-methoxy-3,4-dihydro-2H-pyrido[1,2-b]isoquinoline-1,6-dione (125 mg) in 4 mL pyridine was added hydroxylamine hydrochloride (51 mg). The reaction was heated to reflux for 5 h, then cooled to room temp and partitioned between ether and water. The aqueous solution was extracted with ether (2×). The combined organic solutions were washed with 1 N HCl (1×), and 10% bicarb (1×), then dried (MgSO4) and concentrated. Flash chromatography (10-70% EtOAc/hexanes) gave the titled compound.

WORKUP

后处理

  1. temperatureThe reaction was heated
  2. temperatureto reflux for 5 h
  3. custompartitioned between ether and water
  4. extractionThe aqueous solution was extracted with ether (2×)
  5. washThe combined organic solutions were washed with 1 N HCl (1×), and 10% bicarb (1×)
  6. dry with materialdried (MgSO4)
  7. concentrationconcentrated