反应 #452467
ord-8d6f890a37c14fd4a642ba4963973dd0
反应方程式
propane-1,3-diamine
tetrahydrofuran
pyridine
→
N-(quinolin-2-yl)propane-1,3-diamine
收率 82.0%
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1workup.ADDITIONwas added
- 2温度The reaction mixture was heated
- 3温度at reflux temperature for 18 h
- 4其他To the cooled reaction mixture
- 5过滤the precipitate was filtered off
- 6洗涤washed with tetrahydrofuran (2×50 ml)
- 7其他The solvent was evaporated in vacuo
- 8workup.DISTILLATIONthe residue purified by distillation at 154° C.
实验过程
To a solution of propane-1,3-diamine (65.1 ml, 0.764 mol) in dry pyridine (25 ml) kept under an atmosphere of nitrogen 2-chloro-quinoline (25 g, 0.153 mol) was added. The reaction mixture was heated at reflux temperature for 18 h. To the cooled reaction mixture was added tetrahydrofuran (100 ml) and the precipitate was filtered off and washed with tetrahydrofuran (2×50 ml). The solvent was evaporated in vacuo and the residue purified by distillation at 154° C. and 2.5×10-2 mbar affording 25.34 g (82%) of N-(quinolin-2-yl)propane-1,3-diamine as a crystallising oil.