Thionyl Chloride → N-Methyl 4-Nitrobenzimidoyl Chloride
反応式
[CH3:1][NH:2][C:3](=O)[C:4]1[CH:9]=[CH:8][C:7]([N+:10]([O-:12])=[O:11])=[CH:6][CH:5]=1.S(Cl)([Cl:16])=O>>[CH3:1][N:2]=[C:3]([Cl:16])[C:4]1[CH:9]=[CH:8][C:7]([N+:10]([O-:12])=[O:11])=[CH:6][CH:5]=1参加物
3
実験手順
N-Methyl 4-nitrobenzamide (30.0 g, 167 mmole) and thionyl chloride (256 g, 2.15 mole) were heated at reflux for five hours. The excess thionyl chloride was removed at ~15 mm Hg. Xylene was added to the reaction and distilled under reduced pressure to yield a solid which was recrystallized from petroleum ether to yield 8.6 g of the title compound as a light yellow solid, m.p. 67°-73° C.
後処理
- temperatureat reflux for five hours
- customThe excess thionyl chloride was removed at ~15 mm Hg
- additionXylene was added to the reaction
- distillationdistilled under reduced pressure
- customto yield a solid which
- customwas recrystallized from petroleum ether
出典と根拠
- ORDレコード
- ord-475bb957a2534f33886ec0b0ee0f4e0c
- 出典データセット
- uspto-grants-1985_07
- 特許番号
- US04528382
反応ノート
読み込み中…