HRID989507

反应详情

EQUATION

反应方程式

HRID 989507 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A 100 mL round bottom flask equipped with a magnetic stirrer was charged with (+,−) cis-[2-(4-chloro-phenyl)-cyclopentylamine oxalate salt (200 mg, 0.70 mmol), methylene chloride (5.0 mL) and the solution was cooled to 0° C. DBU (0.84 mL, 5.60 mmol) and isopropylsulfonyl chloride (0.47 mL, 4.20 mmol) were added. The reaction was then stirred at 0° C. for 60.0 minutes and brought to room temperature with stirring overnight. The reaction was diluted with methylene chloride and washed with 1N HCl, brine and the organic layer dried over sodium sulfate. The title compound was purified by radial chromatography eluting with methylene chloride to give 116 mg (55%) of the purified title compound. The nmr was consistent with the assigned structure.

WORKUP

后处理

  1. customA 100 mL round bottom flask equipped with a magnetic stirrer
  2. custombrought to room temperature
  3. stirringwith stirring overnight
  4. washwashed with 1N HCl, brine
  5. dry with materialthe organic layer dried over sodium sulfate
  6. customThe title compound was purified by radial chromatography
  7. washeluting with methylene chloride
  8. customto give 116 mg (55%) of the
  9. custompurified title compound