HRID33537

反应详情

EQUATION

反应方程式

HRID 33537 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

399 mg (10.50 mmol) lithium aluminium hydride were given to 18 ml tetrahydrofuran (THF) and stirred at room temperature (r. t.) for 10 min. A solution of 1.30 g (5.25 mmol) 6-(3-Chloro-phenyl)-pyridine-2-carboxylic acid methyl ester in 18 ml THF was added drop by drop at 0° C. within 15 min., and the mixture stirred for 2 h at 0° C. 32 ml brine were added slowly at 0° C. and stirred continued for 2 h. The mixture was adjusted to pH=5 by slowly addition of conc. HCl. A formed salt precipitate was isolated by filtration and washed with THF. The combined THF-solutions were evaporated, the residue extracted twice with ethyl acetate, the organic phase dried (sodium sulphate) and evaporated. Chromatography on silica (eluent: ethyl acetate/n-heptane 1:1) gave 0.45 g (35%) of [6-(3-Chloro-phenyl)-pyridin-2-yl]-methanol

WORKUP

后处理

  1. stirringthe mixture stirred for 2 h at 0° C
  2. stirringstirred
  3. waitcontinued for 2 h
  4. customA formed salt precipitate was isolated by filtration
  5. washwashed with THF
  6. customThe combined THF-solutions were evaporated
  7. extractionthe residue extracted twice with ethyl acetate
  8. dry with materialthe organic phase dried (sodium sulphate)
  9. customevaporated