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
The product was prepared by procedures which are well known in the art, that is, by the alkylation of 4-nitro-2-methylphenol (2.508 g, 0.0164 mol) with ethyl bromoacetate (3.00 g, 0.018 mol) in acetonitrile (50 mL) in the presence of potassium carbonate (2.76 g) to afford ethyl 4-nitro-2-methylphenoxyacetate (4.0 g, 100%); hydrogenation of the latter (4.0 g, 0.0164 mol) in ethanol (250 mL) in the presence of 10% palladium on carbon (1.0 g) to afford ethyl 4-amino-2-methylphenoxyacetate; which was then dissolved in CH2Cl2 (50 mL) and treated with pyridine (4.0 mL), followed by methanesulfonyl chloride (1.88 g) in CH2Cl2 (5.0 mL) to afford 3.27 g (69.4%) of N-[4-(ethoxycarbonylmethoxy)-3-(methyl)phenyl]methanesulfonamide, m.p. 83°-84° C., after purification by column chromatography on silica.
WORKUP
后处理
- customThe product was prepared by procedures which