HRID1627332
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 3-(3,4-dimethoxyphenyl)-3-methyl-1-nitrobutan-2-ol (700 mg, 2.60 mmol) in DCM (30 mL) were added PCC (3.36 g, 15.60 mmol) and Celite (3.36 g). After stirring 48 h, additional PCC (3.36 g, 15.60 mmol) and Celite (3.36 g) were added. After stirring further for 24 h, the mixture was diluted with Et2O and filtered. The filtrate was concentrated and purified by flash chromatography to afford 3-(3,4-dimethoxyphenyl)-3-methyl-1-nitrobutan-2-one (502 mg, 72%). 1H NMR (400 MHz, CDCl3) δ 6.91-6.84 (m, 2H), 6.69 (s, 1H), 5.13 (s, 2H), 3.90 (s, 3H), 3.89 (s, 3H), 1.56 (s, 6H).
WORKUP
后处理
- stirringAfter stirring further for 24 h
- filtrationfiltered
- concentrationThe filtrate was concentrated
- custompurified by flash chromatography