HRID2081531

反应详情

EQUATION

反应方程式

HRID 2081531 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 2-methoxy-3-cyano-5-ethyl-6-methylpyridine (1.0 g, 5.68 mmol) in dry tetrahydrofuran (50 mL) under a nitrogen atmosphere and cooled to -70° C., was added 1.3M diisobutyl aluminum hydride/THF (17.4 mL, 22.7 mmol). The resulting mixture was allowed to warm to room temperature and stir for 15-20 hours. The reaction mixture was acidified with 1N hydrochloric acid and then neutralized with aqueous sodium bicarbonate. Water was then added and the product extracted into diethyl ether. The etheral extract was dried (Na2SO4), filtered and the solvent evaporated. This residue was flash chromatographed on silica gel eluting with 10% diethyl ether/pentane to give the product.

WORKUP

后处理

  1. extractionthe product extracted into diethyl ether
  2. extractionThe etheral extract
  3. dry with materialwas dried (Na2SO4)
  4. filtrationfiltered
  5. customthe solvent evaporated
  6. customchromatographed on silica gel eluting with 10% diethyl ether/pentane
  7. customto give the product