反応 #60384
ord-e2374bb8c7484fc196589113c5d3c3e8
反応方程式
反応物
試薬
なし
反応条件
詳細条件
See reaction.notes.procedure_details.
後処理
- 1洗浄The organic phase was washed with saturated NaHCO3, water and brine
- 2乾燥dried over Na2SO4
- 3ろ過filtered
- 4濃縮concentrated in vacuo
- 5その他The crude was purified by silica gel chromatography (16-30% EtOAc-hexane)
実験手順
To a solution of 3-phenyl-3-(3-trifluoromethyl-benzenesulfonylamino)-propionic acid (4.31 g, 11.56 mmol), trifluoro-methanesulfonic acid 5-amino-5,6,7,8-tetrahydro-naphthalen-2-yl ester (Step D, 3.10 g, 10.51 mmol), HOBt (Aldrich, 1.28 g, 9.46 mmol), and CH2Cl2 (30 mL) was added EDC (Aldrich, 3.02 g, 15.76 mmol). The reaction was stirred at RT overnight and diluted with CH2Cl2 (100 mL). The organic phase was washed with saturated NaHCO3, water and brine, dried over Na2SO4, filtered and concentrated in vacuo. The crude was purified by silica gel chromatography (16-30% EtOAc-hexane) to afford the title compound as an off-white solid. MS (ESI): 651 (M+H)+.