HRID587628

反应详情

EQUATION

反应方程式

HRID 587628 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
160 °C

PROCEDURE

实验过程

To a solution of compound D6 (0.5 mg, 1.461 mmol) in THF (4 ml), was added hydrazine monohydrate (0.366 g, 7.305 mmol). The reaction mixture was heated at 160° C. under microwave irradiation for 15 min. After cooling, the resulting mixture was concentrated in vacuo. The residue thus obtained was purified by column chromatography (silica gel; DCM/7M solution of NH3 in MeOH up to 3% as eluent). The desired fractions were collected and concentrated in vacuo to yield intermediate compound D7 (0.380 g, 89%) as a white solid.

WORKUP

后处理

  1. temperatureAfter cooling
  2. concentrationthe resulting mixture was concentrated in vacuo
  3. customThe residue thus obtained
  4. customwas purified by column chromatography (silica gel; DCM/7M solution of NH3 in MeOH up to 3% as eluent)
  5. customThe desired fractions were collected
  6. concentrationconcentrated in vacuo