HRID707500

反应详情

EQUATION

反应方程式

HRID 707500 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

To a mixed solution of methyl(2S)-3-(4-(benzyloxy)-2-fluorophenyl)-2-(((9H-fluoren-9-ylmethoxy)carbonyl)amino)propanoate (60.0 g, 114 mmol) described in Production Example 1-2-6 and ethyl acetate (1331 mL) was added lithium iodide (92.0 g, 685 mmol) at room temperature. The resultant mixture was stirred under reflux for 23 hours and 45 minutes. The reaction mixture was cooled to 0° C., and a precipitate was collected by filtration. To the resultant solid was added 1 N hydrochloric acid (228 mL). The resultant solution was extracted with ethyl acetate. An organic layer was dried over anhydrous magnesium sulfate and then filtrated. The solvent was evaporated under a reduced pressure to give the title compound (42.2 g, yield: 72%).

WORKUP

后处理

  1. temperatureunder reflux for 23 hours and 45 minutes
  2. filtrationa precipitate was collected by filtration
  3. additionTo the resultant solid was added 1 N hydrochloric acid (228 mL)
  4. extractionThe resultant solution was extracted with ethyl acetate
  5. dry with materialAn organic layer was dried over anhydrous magnesium sulfate
  6. filtrationfiltrated
  7. customThe solvent was evaporated under a reduced pressure