HRID74298
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 2-(2-(4-methoxycarbonylphenylmethyl)aminonitrobenzen-5-yl)benzoxazole (see Working Example 113-2) (367 mg, 0.910 mmol) was added iron powder (102 mg, 1.82 mmol), 10% aqueous acetic acid (5 mL) and methanol (7 mL), and this was heated to reflux for 16 hours. After the reaction solution was cooled, saturated aqueous sodium hydrogen carbonate solution and chloroform were added, this was filtered through Celite, and the filtrate obtained was extracted. After the organic layer obtained was dried over anhydrous sodium sulfate, it was filtered and concentrated. The residue obtained was purified by silica gel column chromatography to yield the title compound (61.8 mg, 18% yield).
WORKUP
后处理
- temperaturethis was heated
- temperatureto reflux for 16 hours
- temperatureAfter the reaction solution was cooled
- filtrationthis was filtered through Celite
- customthe filtrate obtained
- extractionwas extracted
- customAfter the organic layer obtained
- dry with materialwas dried over anhydrous sodium sulfate, it
- filtrationwas filtered
- concentrationconcentrated
- customThe residue obtained
- customwas purified by silica gel column chromatography