HRID916755
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
A solution of (4-Chloro-7-cyclopentyl-7H-pyrrolo[2,3-d]pyrimidin-5-yl)-(3-nitro-phenyl)-methanone (11.3 g, 30.5 mmol) and NH4OH (200 mL) in 1,4-Dioxane (300 mL) was heated to 50° C. in a pressure reactor. After 2 h the reaction was concentrated under reduced pressure. The residue was dissolved in CH2Cl2 and washed with water. The organic layer was dried over MgSO4 and concentrated to afford the title compound as a yellow solid (10.37 g, 97%). MS: 352.1 (MH+); HPLC Rf: 5.56 min. (HPLC method 4).
WORKUP
后处理
- concentrationAfter 2 h the reaction was concentrated under reduced pressure
- dissolutionThe residue was dissolved in CH2Cl2
- washwashed with water
- dry with materialThe organic layer was dried over MgSO4
- concentrationconcentrated