Toluene → 1-(3-amino-4-chlorophenyl)ethanone
反応式
[CH3:1][C:2]([C:4]1[CH:9]=[CH:8][C:7]([Cl:10])=[C:6]([N+:11]([O-])=O)[CH:5]=1)=[O:3].O.O.Cl[Sn]Cl.C1(C)C=CC=CC=1.[OH-].[Na+]>Cl.CCOCC>[CH3:1][C:2]([C:4]1[CH:9]=[CH:8][C:7]([Cl:10])=[C:6]([NH2:11])[CH:5]=1)=[O:3]参加物
7
実験手順
A mixture of 39.8 g of 4-chloro-3-nitroacetophenone and 136 g of SnCl2.2H2O in 220 ml of concentrated HCl is stirred at room temperature for 0.5 hours. The reaction mixture warms spontaneously to 70° C. then cools. Toluene (200 ml) is added and the reaction mixture is made alkaline with 30% NaOH. Ether is added and the layers are separated. The aqueous layer is extracted twice more with ether, the organic layers are combined, dried, and evaporated. The solid residue is crystallized from benzene to yield 29.6 g of the title compound, melting point 104°-105° C.
後処理
- customwarms spontaneously to 70° C.
- customthe layers are separated
- extractionThe aqueous layer is extracted twice more with ether
- customdried
- customevaporated
- customThe solid residue is crystallized from benzene
出典と根拠
- ORDレコード
- ord-dabe65c3516b4de2a373772155b49dc9
- 出典データセット
- uspto-grants-1982_01
- 特許番号
- US04312990
反応ノート
読み込み中…
