HRID1693162

反应详情

EQUATION

反应方程式

HRID 1693162 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 9H-fluoren-9-ylmethyl ({[(1S*,2R*,4S*)-1-(2-fluorophenyl)-2-(hydroxymethyl)-4-methoxycyclopentyl]amino}carbonothioyl)carbamate (330 mg) in methanol (20 mL)-concentrated hydrochloric acid (1 mL) was heated under reflux for three hours. The reaction solution was concentrated under reduced pressure. Acetonitrile (10 mL) and piperidine (1 mL) were added to the residue at room temperature, and the mixture was stirred at room temperature for one hour. The reaction solution was concentrated under reduced pressure. The resulting crude product was purified by NH-silica gel column chromatography to obtain the title compound (170 mg).

WORKUP

后处理

  1. temperatureunder reflux for three hours
  2. concentrationThe reaction solution was concentrated under reduced pressure
  3. additionAcetonitrile (10 mL) and piperidine (1 mL) were added to the residue at room temperature
  4. concentrationThe reaction solution was concentrated under reduced pressure
  5. customThe resulting crude product was purified by NH-silica gel column chromatography