HRID550037

反应详情

EQUATION

反应方程式

HRID 550037 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A slurry of valsartan barium (90 g) in ethyl acetate (900 ml) and water (360 ml) was treated with hydrochloric acid to attain a pH of about 2 to 2.5. The organic layer was separated, washed with water (3×270 ml) and concentrated at about 45° to 50° C. under reduced pressure. The residue was dissolved in ethyl acetate (225 ml) at 45° to 50° C., filtered at hot condition and cooled to 20° to 25° C. Pentane (900 ml) was then added slowly to the mixture and stirred for 1 hour at 20° to 25° C. The solid obtained was filtered, washed with pentane (2×90 ml) and dried under reduced pressure to obtain the title compound.

WORKUP

后处理

  1. customThe organic layer was separated
  2. washwashed with water (3×270 ml)
  3. concentrationconcentrated at about 45° to 50° C. under reduced pressure
  4. dissolutionThe residue was dissolved in ethyl acetate (225 ml) at 45° to 50° C.
  5. filtrationfiltered at hot condition
  6. temperaturecooled to 20° to 25° C
  7. additionPentane (900 ml) was then added slowly to the mixture
  8. customThe solid obtained
  9. filtrationwas filtered
  10. washwashed with pentane (2×90 ml)
  11. customdried under reduced pressure