HRID1110000

反应详情

EQUATION

反应方程式

HRID 1110000 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 6-(benzyloxy)-α-methyl-1H-benzotriazole-1-acetic acid (36.6 g, 0.123 mole) and concentrated sulfuric acid (2.7 ml) in methanol is stirred at reflux temperature for 6 hours, cooled in an ice bath and treated with K2CO3 (25 g). The resulting mixture is stirred vigorously until a thick slurry results, diluted with methylene chloride and filtered. The filtrate is concentrated in vacuo to give a solid residue. Recrystallization of the residue from methanol affords the title product as a white solid, 27 g, mp 88°-91.5° C., identified by NMR and elemental analyses. Another 4.2 g (81.7% total yield) of the title product is obtained form the mother liquor.

WORKUP

后处理

  1. temperatureat reflux temperature for 6 hours
  2. temperaturecooled in an ice bath
  3. stirringThe resulting mixture is stirred vigorously until a thick slurry
  4. customresults
  5. filtrationfiltered
  6. concentrationThe filtrate is concentrated in vacuo
  7. customto give a solid residue
  8. customRecrystallization of the residue from methanol