HRID352236

反应详情

EQUATION

反应方程式

HRID 352236 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

{[3-(9-Chloro-3-methyl-4-oxo-5H-isoxazolo[4,3-c]quinolin-5-yl)-cyclohexylcarbamoyl]-phenyl-methyl}-carbamic acid tert-butyl ester (1.24 g; 2.2 mmol) was dissolved in excess, neat acetic acid saturated with HCl(g) (20 mL). After stirring 30 min at room temperature, the solution was concentrated to dryness by rotary evaporation. Acetic acid was removed from the resulting solid by consecutive dissolution in, and drying from, acetonitrile (thrice) and then diethyl ether (once). The solid was dissolved in 25% (v/v) isopropyl alcohol in chloroform, washed with saturated NaHCO3(aq), and dried by rotary evaporation to yield the desired product in 97% isolated yield.

WORKUP

后处理

  1. concentrationthe solution was concentrated to dryness by rotary evaporation
  2. customAcetic acid was removed from the resulting solid by consecutive dissolution in, and
  3. dry with materialdrying from, acetonitrile (thrice)
  4. dissolutionThe solid was dissolved in 25% (v/v) isopropyl alcohol in chloroform
  5. washwashed with saturated NaHCO3(aq)
  6. customdried by rotary evaporation