HRID8683

反应详情

EQUATION

反应方程式

HRID 8683 的结构方程式

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

  1. customseparate reactions
  2. customrespectively, essentially as described above in example 18 except that the reaction mixtures
  3. filtrationare filtered through 2 g of silica (ethyl acetate
  4. concentrationCombine and concentrate the appropriate fractions
  5. customPurify by column chromatography on silica gel
  6. washElute the column with a step gradient of 50% ethyl acetate in heptane to 100% ethyl acetate