HRID8683
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
The title compound is prepared from 3-[3-(2-bromo-ethoxy)-phenyl]-thieno[2,3-d]isoxazole, potassium carbonate, and benzylamine in two separate reactions using acetonitrile and 90% aqueous acetonitrile, respectively, essentially as described above in example 18 except that the reaction mixtures are filtered through 2 g of silica (ethyl acetate then dichloromethane). Combine and concentrate the appropriate fractions. Purify by column chromatography on silica gel. Elute the column with a step gradient of 50% ethyl acetate in heptane to 100% ethyl acetate to give the title compound (0.350 g, 81%). mp=60–63° C. Microanalysis (C, H, N) is consistent with the final compound.
WORKUP
后处理
- customseparate reactions
- customrespectively, essentially as described above in example 18 except that the reaction mixtures
- filtrationare filtered through 2 g of silica (ethyl acetate
- concentrationCombine and concentrate the appropriate fractions
- customPurify by column chromatography on silica gel
- washElute the column with a step gradient of 50% ethyl acetate in heptane to 100% ethyl acetate