HRID272693
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
4-Chloro-2-methoxy-benzaldehyde (0.54 g, 3.2 mmol) in 10 mL of THF was treated with 3.0 M EtMgBr (2 mL, 6.0 mmol) at room temperature. The solution was stirred for 1 hour and quenched with MeOH. The solution was poured into water, treated 10 mL of 10% HCl, extracted with EtOAc several times. The combined organic layers were washed brine, dried (MgSO4), filtered, and concentrated. The residue was diluted with CH2Cl2, treated with PCC (1.33 g, 6.4 mmol) for 2 hours. The reaction mixture was filtered through a pack of silica gel to give 0.42 g of the title compound. MS (DCI) m/e 199 (M+H)+.
WORKUP
后处理
- customquenched with MeOH
- additionThe solution was poured into water
- additiontreated 10 mL of 10% HCl
- extractionextracted with EtOAc several times
- washThe combined organic layers were washed brine
- dry with materialdried (MgSO4)
- filtrationfiltered
- concentrationconcentrated
- additionThe residue was diluted with CH2Cl2
- filtrationThe reaction mixture was filtered through a pack of silica gel