HRID639792

反应详情

EQUATION

反应方程式

HRID 639792 反应方程式

CONDITIONS

反应条件

温度
160 °C

PROCEDURE

实验过程

A mixture of 1,3-diazepan-2-one hydrazone hydroiodide (1.00 g, 3.9 mmol) and isonicotinoyl chloride hydrochloride (695 mg, 3.9 mmol) was heated in a microwave reactor at 160° C. for 10 min. The reaction mixture was poured into NaaCO3 solution, sat., and extracted with DCM. The organic phase was dried and concentrated. Flash chromatography (DCM/MeOH 20:1) gave 1.74 g crude title compound which was used directly in the next step. 1H NMR: 1.89 (s, 4H) 3.15 (m, 2H) 3.86 (m, 2H) 7.44 (d, 2H) 8.66 (d, 2H).

WORKUP

后处理

  1. additionThe reaction mixture was poured into NaaCO3 solution
  2. extractionsat., and extracted with DCM
  3. customThe organic phase was dried
  4. concentrationconcentrated