HRID6079
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
A solution of compound of Step 6 (0.926 g, 2.85 mmol) and trifluoroacetic acid (5.49 mL, 71.3 mmol) in CH2Cl12 (5.49 mL) was stirred at room temperature for 30 minutes and then concentrated in vacuo. The residue was dissolved in 1.0N KOH (7 mL) and extracted with ethyl acetate (4×10 mL). The combined organic layers were dried over MgSO4 and then concentrated to give the title amine as an off-white solid (0.67 g, 100% yield). 1H and 13C NMR spectral data were consistent with the proposed structure.
WORKUP
后处理
- concentrationconcentrated in vacuo
- dissolutionThe residue was dissolved in 1.0N KOH (7 mL)
- extractionextracted with ethyl acetate (4×10 mL)
- dry with materialThe combined organic layers were dried over MgSO4
- concentrationconcentrated