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
3-(3,4-Dimethoxy-phenyl)-1H-pyrrolo-[2,3-b]pyridine 1 (50 mg, 0.20 mmol) was dissolved in N,N-dimethylformamide (4 mL). Sodium hydride (10 mg, 0.24 mmol, 60% dispersion in mineral oil) was added. The reaction mixture was stirred for 15 minutes at room temperature. 1-Isothiocyanatobenzene (35 μL, 0.29 mmol) was added and the reaction mixture was stirred for 40 minutes at room temperature. The product was concentrated and the residue was partitioned between brine and ethyl acetate. The organic portion was dried over anhydrous sodium sulfate, filtered, and concentrated to provide a solid. The solid was washed with a minimum of methanol and dried in vacuo to provide 41, (38 mg, 49%). MS(ESI) [M+H+]+=390.2.
WORKUP
后处理
- stirringthe reaction mixture was stirred for 40 minutes at room temperature
- concentrationThe product was concentrated
- customthe residue was partitioned between brine and ethyl acetate
- dry with materialThe organic portion was dried over anhydrous sodium sulfate
- filtrationfiltered
- concentrationconcentrated
- customto provide a solid
- washThe solid was washed with a minimum of methanol
- customdried in vacuo