反応 #73939
ord-778d7f5e63f94085bc1bae2701c3a430
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washed with NaHCO3 (50 mL)
- 2抽出The aqueous layer was extracted with DCM (2×50 mL)
- 3洗浄the combined organic fractions washed with water (200 mL), brine (200 mL)
- 4乾燥dried over Na2SO4
- 5その他Removing the solvent
実験手順
To a solution of 3-(6,8-dichloro-2-methyl-1,2,3,4-tetrahydroisoquinolin-4-yl)benzene-1-sulfonyl chloride (intermediate 1.6) (600 mg, 1.41 mmol) in chloroform (2.82 mL) was added DIEA (545.7 mg, 4.24 mmol) and 2-(2-(2-(2-azidoethoxy)ethoxy)ethoxy)ethanamine (616.3 mg, 2.82 mmol). The reaction was stirred overnight at which point the mixture was diluted with 50 mL DCM and washed with NaHCO3 (50 mL). The aqueous layer was extracted with DCM (2×50 mL) and the combined organic fractions washed with water (200 mL), brine (200 mL), and dried over Na2SO4. Removing the solvent gave the title compound as an oil which was used without further purification.