HRID1791047
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
1.12 g (4.07 mmol) of 4-(4,6-dimethoxy-1,3,5-triazin-2-yl)-4-methylmorpholinium chloride and then 0.379 g (4.07 mmol) of aniline are successively added to 0.75 g (3.7 mmol) of 3-methylene-2,3-dihydro-1-benzoxepin-7-carboxylic acid, prepared according to example 40, in solution in 25 ml of methanol. The medium is stirred at ambient temperature for 24 h. After evaporating the methanol, the crude reaction product is purified by chromatography on silica gel (ethyl acetate/heptane 40/60) to give 185 mg (49%) of 3-methylene-N-phenyl-2,3-dihydro-1-benzoxepin-7-carboxamide in the form of a pink solid; M.p.=139° C.
WORKUP
后处理
- customprepared
- customAfter evaporating the methanol
- customthe crude reaction product
- customis purified by chromatography on silica gel (ethyl acetate/heptane 40/60)