HRID1613639

反应详情

EQUATION

反应方程式

HRID 1613639 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

20 g (0.068 mol) of 1-(pyrid-3-yl)-2-(2-bromophenyl)-2-hydroxyethanone in 300 ml of methanol were reduced with 3 g (0.079 mol) of sodium borohydride at 0° C. Stirring was carried out for a few hours at room temperature (21° C.), the pH was brought to 2 with 4N hydrochloric acid and 4 ml of ethylene glycol were added. The solution was evaporated down, after which the residue was covered with a layer of ethyl acetate and neutralized with NaHCO3 solution. The ethyl acetate phase was washed twice with water and dried over Na2SO4. After the ethyl acetate had been distilled off, the product was obtained as a white powder of melting point 115° C.

WORKUP

后处理

  1. waitwas carried out for a few hours at room temperature
  2. custom(21° C.)
  3. additionwere added
  4. customThe solution was evaporated down
  5. washThe ethyl acetate phase was washed twice with water
  6. dry with materialdried over Na2SO4
  7. distillationAfter the ethyl acetate had been distilled off
  8. customthe product was obtained as a white powder of melting point 115° C.