HRID1678736
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 [2-(4-[1,3]dioxolan-2-yl-phenyl)-3-phenyl-[1,6]naphthyridin-5-yl]-hydrazine (3-4, 5.3 g, 13.8 mmol) in CH2Cl2 (anhydrous, 40 mL) at 0° C. was added triethylamine (9.7 mL, 68.9 mmol) followed by a rapid addition of phosgene in toluene (2M, 7.6 mL). After stirring for 10 min at room temperature, the mixture was concentrated and water (30 mL) was added. The solid was collected and dried with toluene azeotropically to give the title compound which was used for the next step without further purification. LRMS m/z (M+1) Calcd: 411.1. Found 411.2.
WORKUP
后处理
- concentrationthe mixture was concentrated
- additionwater (30 mL) was added
- customThe solid was collected
- dry with materialdried with toluene azeotropically