HRID2102293

反应详情

EQUATION

反应方程式

HRID 2102293 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

Me3OBF4 (2.66 g, 18 mmol) was added to a solution of 2-pyrollidinone in DCM (150 ml) and the reaction mixture was stirred for 24 h. The reaction mixture was washed with aq. sat. NaHCO3, dried and concentrated. The residue was dissolved in EtOH (4 ml) and isonicotinic hydrazide (1.37 g, 10 mmol) was added. The mixture was heated in a microwave reactor for 1 h at 120° C. The volatiles were removed and the crude product purified with column chromatography (DCM/MeOH 20:1) to give 319 mg (11%) of the title compound. 1H NMR: 2.87 (m, 2H), 3.05 (t, 2H), 4.28 (t, 2H), 7.72 (d,2H), 8.72 (d, 2H).

WORKUP

后处理

  1. washThe reaction mixture was washed with aq. sat. NaHCO3
  2. customdried
  3. concentrationconcentrated
  4. dissolutionThe residue was dissolved in EtOH (4 ml)
  5. customThe volatiles were removed
  6. customthe crude product purified with column chromatography (DCM/MeOH 20:1)