4-Nitrobenzoyl chloride → 2-(4-Nitrophenyl)Benzo[D]Thiazole
反応式
[N+:1]([C:4]1[CH:12]=[CH:11][C:7]([C:8](Cl)=O)=[CH:6][CH:5]=1)([O-:3])=[O:2].[NH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=1[SH:20]>C1C=CC=CC=1>[N+:1]([C:4]1[CH:12]=[CH:11][C:7]([C:8]2[S:20][C:15]3[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=3[N:13]=2)=[CH:6][CH:5]=1)([O-:3])=[O:2]参加物
4
実験手順
A solution of 4-nitrobenzoyl chloride (1.49 g, 8.0 mmol) in benzene (anhydrous, 10 mL) was added dropwise to 2-aminothiophenol (1.0 g, 8.0 mmol in 10 ml of benzene) at room temperature. The reaction mixture was allowed to stir for 16 hr. The reaction was quenched with water (20 mL). The aqueous layer was separated and extracted with ethyl acetate (3×10 ml). The combined organic layers were dried and evaporated. The crude product was purified with flush column, (hexane:ethyl acetate=85:15) to give 1.5 g (73.2%) of product as light yellow solid.
後処理
- customThe reaction was quenched with water (20 mL)
- customThe aqueous layer was separated
- extractionextracted with ethyl acetate (3×10 ml)
- customThe combined organic layers were dried
- customevaporated
- customThe crude product was purified
- customwith flush column, (hexane:ethyl acetate=85:15)
出典と根拠
- ORDレコード
- ord-2be7382ca6aa42e68bb6b2793932295f
- 出典データセット
- uspto-grants-2014_12
- 特許番号
- US08911707B2
反応ノート
読み込み中…