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
A recovery flask was charged with 520 mg (2.81 mmol) of the optically active 1-(4-fluorophenyl)-2-nitroethanol obtained in Example 14, 52 mg of 10% Pd/C, and 2.8 ml of methanol, and stirring was carried out under an atmosphere of hydrogen at atmospheric pressure and 30° C. for 22 hours. After the reaction was completed, the catalyst was filtered off and the solvent was distilled off under vacuum to give 421 mg (yield 97%, 1H-NMR) of optically active 2-amino-1-(4-fluorophenyl)ethanol as white crystals. The amino group of the amino alcohol so obtained was monobenzoylated by reaction with benzoyl chloride, and when it was analyzed using a CHIRALCEL OD column (eluant; n-hexane:2-propanol=30:1), it was found that the optical purity was 96% ee.
WORKUP
后处理
- filtrationthe catalyst was filtered off
- distillationthe solvent was distilled off under vacuum