HRID412069

反应详情

EQUATION

反应方程式

HRID 412069 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 the compound of Example 1 (50.0 mg, 129 μmol) in dichloromethane (2 ml) was added phenyl isocyanate (46.2 mg, 388 μmol), and the mixture was stirred overnight at room temperature. Diisopropyl ether was added to the reaction mixture, and the precipitated crystals were collected by filtration and air-dried. These were dissolved into acetic acid (5 ml) and concentrated hydrochloric acid (1 ml) was added, which was stirred overnight at room temperature. The reaction mixture was concentrated under reduced pressure. The residue was washed with water and ethyl acetate in sequence and then air-dried, thereby obtaining 41.0 mg of title compound as yellow powder. Yield 71%.

WORKUP

后处理

  1. filtrationthe precipitated crystals were collected by filtration
  2. customair-dried
  3. dissolutionThese were dissolved into acetic acid (5 ml) and concentrated hydrochloric acid (1 ml)
  4. additionwas added
  5. stirringwhich was stirred overnight at room temperature
  6. concentrationThe reaction mixture was concentrated under reduced pressure
  7. washThe residue was washed with water and ethyl acetate in sequence
  8. customair-dried