HRID1850236

反应详情

EQUATION

反应方程式

HRID 1850236 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
127.5 °C

PROCEDURE

实验过程

A mixture of (S)-3-(2-chloro-5-fluoropyrimidin-4-yl)-4-phenyloxazolidin-2-one (40 mg, 0.136 mmol), (S)-1-cyclopropylethanamine (34.8 mg, 0.409 mmol), Hunig's Base (0.119 mL, 0.681 mmol) in DMSO (0.4 mL) was heated under argon at 105-115° C. for ˜18 hrs (alternative: 120-135° C. for ˜90 min). Then mixture was allowed to cool to room temperature. The mixture was diluted with DMSO and water (˜10 vol. % of DMSO), filtered through a syringe filter and purified by reverse phase HPLC. Selected fractions were collected and lyophilized providing (S)-3-(2-((S)-1-cyclopropylethylamino)-5-fluoropyrimidin-4-yl)-4-phenyloxazolidin-2-one (26 mg) as a white solid as its trifluoroacetic acid salt.

WORKUP

后处理

  1. temperatureto cool to room temperature
  2. filtrationfiltered through a syringe
  3. filtrationfilter
  4. custompurified by reverse phase HPLC
  5. customSelected fractions were collected