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
反応条件
- 温度
- 10 °C
実験手順
Combine 5-[(dimethylamino)methyl]-furfuryl alcohol hydrochloride (1.72 kg, 8.97 mol) and acetonitrile (4.3 L). Cool to about 10° C. Add thionyl chloride (1.02 kg, 8.54 mol) dropwise, while maintaining the temperature of the reaction at below about 40° C. After the addition of thionyl chloride is complete, add methanesulfonic acid (1.3 kg, 13.5 mol). Distill to remove about 1.8 L of distillate to give the title compound as a solution.
後処理
- customthe temperature of the reaction at below about 40° C
- distillationDistill
- customto remove about 1.8 L of distillate
出典と根拠
- ORDレコード
- ord-82f011ea3df240f298bd03a1f2836efc
- 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…