HRID1009265
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of the fluoro derivative (21.0 g) from Step 4 in 90% aqueous ethyl alcohol (216 μL) was added potassium hydroxide (21.9 g). The mixture was heated at reflux for 4 hours and cooled to room temperature. The mixture was then concentrated and co-evaporated with toluene (3×300 mL). The residue was dissolved in dichloromethane (500 mL) and stirred for 0.5 hour. The suspension was filtered through celite and the celite was washed with dichloromethane (3×100 mL). The filtrate was concentrated to dryness to yield (2S)-2-amino-4-fluoro-4-methylpentan-1-ol.
WORKUP
后处理
- temperatureThe mixture was heated
- temperatureat reflux for 4 hours
- concentrationThe mixture was then concentrated
- dissolutionThe residue was dissolved in dichloromethane (500 mL)
- filtrationThe suspension was filtered through celite
- washthe celite was washed with dichloromethane (3×100 mL)
- concentrationThe filtrate was concentrated to dryness