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
Methyl 2-(1-methylpyrrol-2-yl)-2-(4-nitrophenyl)acetate (9.2 g, 33.54 mmol) [prepared as in Example 21, Step (a)], was dissolved in methanol (100 ml) and an aqueous solution of lithium hydroxide (3.52 g in 50 ml of water) was added. After 1.5 h the reaction mixture was concentrated to dryness in vacuo and the resulting residue was dissolved in water (100 ml). The solution was acidified to pH 1 with 6 M HCl and then extracted with ethyl acetate. The organic extracts were washed with water, and brine, and dried over magnesium sulfate. The solvent was removed in vacuo and the residue was purified by flash chromatography (hexane-ethyl acetate, 9:1) to give 4-(1-methylpyrrol-2-ylmethyl)nitrobenzene (4.8 g, 66%) as a yellow oil. ##STR62##
WORKUP
后处理
- concentrationAfter 1.5 h the reaction mixture was concentrated to dryness in vacuo
- dissolutionthe resulting residue was dissolved in water (100 ml)
- extractionextracted with ethyl acetate
- washThe organic extracts were washed with water, and brine
- dry with materialdried over magnesium sulfate
- customThe solvent was removed in vacuo
- customthe residue was purified by flash chromatography (hexane-ethyl acetate, 9:1)