HRID1714416

反应详情

EQUATION

反应方程式

HRID 1714416 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a stirred solution of dimethyl 2-[(6-chloropyridin-3-yl)methyl]-2-methylmalonate (10.85 g, 40 mmol) in THF (80 mL) was added a solution of lithium hydroxide monohydrate (5.7 g, 0.136 mol) in water (43 mL). The resulting mixture was stirred overnight at room temperature and then poured into water (300 mL). The pH was adjusted to less than 2 by the addition of concentrated HCl. The resulting mixture was extracted with ether (3×100 mL) and the ether extracts were combined, washed with brine (100 mL) and dried over anhydrous MgSO4. After a filtration, the solvent was evaporated to give 9.26 g of the product as a white solid in 95% yield: m.p. 168° C. (decomp.).

WORKUP

后处理

  1. extractionThe resulting mixture was extracted with ether (3×100 mL)
  2. washwashed with brine (100 mL)
  3. dry with materialdried over anhydrous MgSO4
  4. filtrationAfter a filtration
  5. customthe solvent was evaporated