Trimethylsilyldiazomethane → Methyl 4-amino-3-bromo-5-nitrobenzoate
反応式
[NH2:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][C:3]=1[Br:14].[CH3:15][Si](C=[N+]=[N-])(C)C>ClCCl.CO>[NH2:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][C:5]([C:6]([O:8][CH3:15])=[O:7])=[CH:4][C:3]=1[Br:14]参加物
5
実験手順
To a solution of 4-amino-3-bromo-5-nitrobenzoic acid (3.65 g, 14.0 mmol) in dichloromethane (35 mL) and methanol (35 mL) at 0° C. was slowly added trimethylsilyl-diazomethane (8.74 mL, 17.5 mmol). The mixture was allowed to warm to ambient temperature and concentrated. Purification by silica gel chromatography (100% hexanes→50% hexanes/ethyl acetate) gave the title compound (1.54 g). LC-MS [M]=275.1.
後処理
- customat 0° C.
- concentrationconcentrated
- customPurification by silica gel chromatography (100% hexanes→50% hexanes/ethyl acetate)
出典と根拠
- ORDレコード
- ord-4f3a9c84fc614cf98f51713fec7f35d5
- 出典データセット
- uspto-grants-2016_01
- 特許番号
- US09238647B2
反応ノート
読み込み中…