Hydrochloric Acid → 1-Methyl-1,2,3,6-tetrahydropyridin-1-ium-5-carboxylic acid;chloride
反応式
[CH3:1][N:2]1[CH2:7][C:6]([C:8]([O:10]C)=[O:9])=[CH:5][CH2:4][CH2:3]1.[ClH:12].Cl>C(O)C>[CH3:1][NH+:2]1[CH2:7][C:6]([C:8]([OH:10])=[O:9])=[CH:5][CH2:4][CH2:3]1.[Cl-:12]参加物
4
反応条件
- 温度
- 100 °C
実験手順
In a 250 ml flask equipped with a magnetic stirrer and a condenser, arecoline hydrochloride (4 g; 20.9 mmol) is added to a solution of 50 ml of 95% ethanol and 60 ml of concentrated HCl. The mixture is heated at 100° C. for 12 hours then at reflux for 6 hours. The solvents are evaporated off under reduced pressure leaving a solid residue. The residue is recrystallized from a 95% ethanol/ether mixture in order to produce 1.69 g of product (Yield=46%) in the form of white crystals.
後処理
- customIn a 250 ml flask equipped with a magnetic stirrer and a condenser
- temperatureat reflux for 6 hours
- customThe solvents are evaporated off under reduced pressure
- customleaving a solid residue
- customThe residue is recrystallized from a 95% ethanol/ether mixture in order
出典と根拠
- ORDレコード
- ord-fad818f96b7040cabd0e588cf5e3fc47
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07745413B2
反応ノート
読み込み中…