Methanesulfonic Acid → 5-Dimethylaminomethylfurfuryl chloride hydrochloride
反応式
[ClH:1].[CH3:2][N:3]([CH2:5][C:6]1[O:12][C:9]([CH2:10]O)=[CH:8][CH:7]=1)[CH3:4].S(Cl)([Cl:15])=O.CS(O)(=O)=O>C(#N)C>[ClH:15].[CH3:2][N:3]([CH2:5][C:6]1[O:12][C:9]([CH2:10][Cl:1])=[CH:8][CH:7]=1)[CH3:4]参加物
5
実験手順
Combine 5-[(dimethylamino)methyl]-furfuryl alcohol hydrochloride (201 g, 1.05 mol) and acetonitrile (500 mL). Add dropwise, thionyl chloride (119 g, 1.0 mol) at such a rate that the temperature of the reaction is maintained at about 30° C. to 35° C. After the addition of thionyl chloride is complete, add methanesulfonic acid (144 g, 1.5 mol) while removing sulfur dioxide and acetonitrile by distillation. Stop the distillation when about 250 mL of distillate has been collected to give the title compound as a solution.
後処理
- additionAdd dropwise
- customwhile removing sulfur dioxide and acetonitrile
- distillationby distillation
- distillationthe distillation when about 250 mL of distillate
- customhas been collected
出典と根拠
- ORDレコード
- ord-88d0520323934382803a9e351b4cb7bb
- 出典データセット
- uspto-grants-1997_09
- 特許番号
- US05672724
反応ノート
読み込み中…