HRID49548

反应详情

EQUATION

反应方程式

HRID 49548 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-{4-[3-[1(S)-(4-Chlorophenyl)ethyl]1-(4-cyclohexylphenyl)ureidomethyl]benzoyl-amino}propionic acid methyl ester (1.1 g, 1.9 mmol) was dissolved in methanol (10 ml) and 1N aqueous sodium hydroxide (5.7 ml) was added. The reaction mixture was stirred at room temperature for 2 hours. Then 1N hydrochloric acid was added and the solvent was removed by rotary evaporation in vacuo. The residue was re-dissolved in ethyl acetate and diethyl ether and crystallised using sonication. Concentration in vacuo followed by re-suspension in a aqueous hydrochloric acid and sinication for 30 min afforded after filtration, washing with water and drying in vacuo 0.55 g (51%) of the title compound as a solid.

WORKUP

后处理

  1. customthe solvent was removed by rotary evaporation in vacuo
  2. dissolutionThe residue was re-dissolved in ethyl acetate
  3. customdiethyl ether and crystallised
  4. customsonication
  5. concentrationConcentration in vacuo
  6. waitfollowed by re-suspension in a aqueous hydrochloric acid and sinication for 30 min
  7. customafforded
  8. filtrationafter filtration
  9. washwashing with water
  10. dry with materialdrying in vacuo 0.55 g (51%) of the title compound as a solid