HRID2169273

反应详情

EQUATION

反应方程式

HRID 2169273 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 5-benzyloxy-2-[1-(4-bromophenyl)-cyclopentylmethyl]-6-hydroxypyrimidine-4-carboxylic acid tert-butyl ester (230) (7.9 g, 14.64 mmol) in tetrahydrofuran (200 mL) was added an aqueous solution (100 mL) of LiOH.H2O (6.15 g, 146.44 mmol). The resulting mixture was refluxed for 16 h. After completion of the reaction the organic solvent was removed on a rotary evaporator and water (30 mL) was added. The aqueous solution was acidified (pH 5) with concentrated HCl at 0° C. to give a white solid which was filtered off. The solid residue was triturated in diethyl ether and filtered. After drying, 5-benzyloxy-2-[1-(4-bromophenyl)-cyclopentylmethyl]-6-hydroxypyrimidine-4-carboxylic acid (231) was obtained (6.3 g, 89%) as a white solid.

WORKUP

后处理

  1. temperatureThe resulting mixture was refluxed for 16 h
  2. customAfter completion of the reaction the organic solvent
  3. customwas removed on a rotary evaporator and water (30 mL)
  4. additionwas added
  5. customat 0° C.
  6. customto give a white solid which
  7. filtrationwas filtered off
  8. customThe solid residue was triturated in diethyl ether
  9. filtrationfiltered
  10. customAfter drying