Sodium Hydroxide → 3,5-Diaminobenzonitrile
反応式
[N+:1]([C:4]1[CH:5]=[C:6]([CH:9]=[C:10]([N+:12]([O-])=O)[CH:11]=1)[C:7]#[N:8])([O-])=O.Cl[Sn]Cl.[OH-].[Na+]>Cl>[NH2:1][C:4]1[CH:5]=[C:6]([CH:9]=[C:10]([NH2:12])[CH:11]=1)[C:7]#[N:8]参加物
5
実験手順
To 3,5-dinitrobenzonitrile (5.0 g, 25.89 mmol) in 20 mL of HCl 1M, was added SnCl2 (34.4 g, 7 eq). The reaction mixture was stirred at room temperature for 2 h and then cooled to 0° C. The mixture was made alkaline with a 50% aqueous solution of NaOH and the precipitate was removed by filtration. The filtrate was extracted with ethyl acetate and the combined organic layers were evaporated. The residue and the precipitate were purified by flash chromatography on silica gel (DCM/MeOH//95/5) to yield expected compound as an orange solid (1.95 g, 57% yield). m/z (ESI) 134.0 [M+H]+.
後処理
- temperaturecooled to 0° C
- customthe precipitate was removed by filtration
- extractionThe filtrate was extracted with ethyl acetate
- customthe combined organic layers were evaporated
- customThe residue and the precipitate were purified by flash chromatography on silica gel (DCM/MeOH//95/5)
出典と根拠
- ORDレコード
- ord-c9d06e2ce5ab4de282e6822838a95cc4
- 出典データセット
- uspto-grants-2014_03
- 特許番号
- US08680095B2
反応ノート
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