Hydrazine → 3-Bromo-4-chlorobenzhydrazide
反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH:9]=[CH:10][C:11]=1[Cl:12])[C:5](OC)=[O:6].[NH2:13][NH2:14]>CO>[Br:1][C:2]1[CH:3]=[C:4]([CH:9]=[CH:10][C:11]=1[Cl:12])[C:5]([NH:13][NH2:14])=[O:6]参加物
4
反応条件
- 温度
- 70 °C
実験手順
Methyl 3-bromo-4-chlorobenzoate (120 mg, 0.481 mmol) was added to hydrazine (23.12 mg, 0.721 mmol) in methanol (8 mL) and refluxed for 12 h at 70° C. Reaction was monitored by TLC. After completion of the reaction, the solvent was removed by vacuum and then compound was purified by column chromatography affording the title compound (30 mg). 1H NMR (400 MHz, CDCl3): δ 8.02 (d, 1H, J=1.6 Hz), 7.60 (dd, 1H, J=2.0 & 8.0 Hz), 7.52 (d, 1H, J=8.0 Hz), ESI-MS: 250.9 [M+H]+.
後処理
- customReaction
- customAfter completion of the reaction
- customthe solvent was removed by vacuum
- customcompound was purified by column chromatography
出典と根拠
- ORDレコード
- ord-9b1e46968d694f988be8325407bdd3ba
- 出典データセット
- uspto-grants-2015_03
- 特許番号
- US08987335B2
反応ノート
読み込み中…