HRID2252036
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-phenyl-6,7-dihydro-5H-pyrrolo[1,2-a]imidazole (3.38 g, 18.3 mmol) in dry CH2Cl2 (113 mL) slowly add bromine (1.0 mL, 20.2 mmol) and stir the mixture at room temperature for 1.5 hours. Add a saturated aqueous solution of NaHCO3 (100 mL) and extract with CH2Cl2 (3×100 mL). Wash the combined organic layers with NaHSO3 (40%, 30 mL), dry (MgSO4) and concentrate in vacuo. Purify the residue by flash chromatography (SiO2, eluent: CH2Cl2 to CH2Cl2/MeOH 20:1) to yield a red solid, 3.54 g, 73% yield. MS(ES+): m/z=263.0 (M+H)+
WORKUP
后处理
- extractionextract with CH2Cl2 (3×100 mL)
- washWash the combined organic layers with NaHSO3 (40%, 30 mL)
- dry with materialdry (MgSO4)
- concentrationconcentrate in vacuo
- customPurify the residue by flash chromatography (SiO2, eluent: CH2Cl2 to CH2Cl2/MeOH 20:1)
- customto yield a red solid, 3.54 g, 73% yield