HRID412069
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- filtrationthe precipitated crystals were collected by filtration
- customair-dried
- dissolutionThese were dissolved into acetic acid (5 ml) and concentrated hydrochloric acid (1 ml)
- additionwas added
- stirringwhich was stirred overnight at room temperature
- concentrationThe reaction mixture was concentrated under reduced pressure
- washThe residue was washed with water and ethyl acetate in sequence
- customair-dried