HRID554018

反应详情

EQUATION

反应方程式

HRID 554018 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

4-(1-Hydroxy-1-methylethyl)-2-propyl-1H-imidazole-5-carboxylic acid ethyl ester (100 g), N-(triphenylmethyl)-5-(4′-bromomethyl biphenyl-2-yl)tetrazole (250 g), potassium carbonate (170 g) & tetra butyl ammonium bromide (15 g) in acetone (2.5 L) were refluxed for 10-16 hours. Progress of reaction was monitor by HPLC. After completion of reaction, reaction mass was cooled and filtered to remove the salts. Inorganic salts were washed with acetone (300 mL). Acetone from combine the filtrate and washings was distilled. The residue obtained was crystallized in acetonitrile to get ethyl-4-(1-hydroxy-1-methylethyl)-2-propyl-1-{4-[2-(trityltetrazol-5-yl)phenyl]phenyl}methylimidazole-5-carboxylate (280 g).

WORKUP

后处理

  1. customProgress of reaction
  2. customAfter completion of reaction, reaction mass
  3. temperaturewas cooled
  4. filtrationfiltered
  5. customto remove the salts
  6. washInorganic salts were washed with acetone (300 mL)
  7. distillationAcetone from combine the filtrate and washings was distilled
  8. customThe residue obtained
  9. customwas crystallized in acetonitrile