HRID6374

反应详情

EQUATION

反应方程式

HRID 6374 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of NaOH (0.488 g) in 10 ml of H2O was added 5 ml of 95% ethanol, followed by 3-benzyloxyacetophenone (2.5 g). The resulting solution was cooled to 0°-5° C. and pyridine-3-carbaldehyde (0.903 ml) added. After standing at 0°-5° C. for 18 hours, present title product was recovered by filtration and purified by chromatography on silica gel using 1:4 ethyl acetate:CH2Cl2 as eluant to yield 1.5 g of purified title product as an off-white solid; mp 117°-119° C.; IR (KBr) 1660 cm-1;Anal. C 79.83, H 5.50, N 4.22, calcd. C 79.98, H 5.43, N 4.44.

WORKUP

后处理

  1. temperatureThe resulting solution was cooled to 0°-5° C.
  2. filtrationpresent title product was recovered by filtration
  3. custompurified by chromatography on silica gel using 1:4 ethyl acetate
  4. customCH2Cl2 as eluant to yield 1.5 g
  5. customof purified title product as an off-white solid