反応式
[Cl:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[C:9]([Cl:14])[C:8]([F:15])=[CH:7][C:3]=1[C:4](O)=[O:5].S(Cl)([Cl:18])=O>>[Cl:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[C:9]([Cl:14])[C:8]([F:15])=[CH:7][C:3]=1[C:4]([Cl:18])=[O:5]参加物
3
実験手順
106.6 g of 2,4-dichloro-5-fluoro-3-nitro-benzoic acid are heated at the boiling point under reflux with 250 ml of thionyl chloride for 2 hours. The excess thionyl chloride is then distilled off under normal pressure and the residue is fractionated under a fine vacuum. 104.7 g of 2,4-dichloro-5-fluoro-3-nitro-benzoyl chloride pass over at 110°-115° C./0.08-0.09 mbar. On standing, crystals of melting point 35°-37° C. form.
後処理
- distillationThe excess thionyl chloride is then distilled off under normal pressure
- customover at 110°-115° C./0.08-0.09 mbar
出典と根拠
- ORDレコード
- ord-a607af53d6a74582a8a1138320f1a937
- 出典データセット
- uspto-grants-1991_01
- 特許番号
- US04981854
関連ノート
読み込み中…