Trimethylsilyldiazomethane → Methyl 2-amino-4-bromo-3-methylbenzoate
反応式
[CH3:1][Si](C=[N+]=[N-])(C)C.[NH2:8][C:9]1[C:17]([CH3:18])=[C:16]([Br:19])[CH:15]=[CH:14][C:10]=1[C:11]([OH:13])=[O:12]>C(OCC)(=O)C.C(O)C>[NH2:8][C:9]1[C:17]([CH3:18])=[C:16]([Br:19])[CH:15]=[CH:14][C:10]=1[C:11]([O:13][CH3:1])=[O:12]参加物
5
実験手順
Add (trimethylsilyl)diazomethane (16.5 mL, 33 mmol, 2 M in hexane) to a solution of 2-amino-4-bromo-3-methyl-benzoic acid (3.8 g, 16.5 mmol) in ethyl acetate (50 mL) and ethanol (50 mL) at room temperature and stir the solution for 16 h. Remove the solvent under reduced pressure. Chromatograph the residue over silica gel, eluting with hexanes/ethyl acetate, to afford the title compound (3.54 g, 88%). MS (ES+): 245 (M+H).
後処理
- customRemove the solvent under reduced pressure
- washChromatograph the residue over silica gel, eluting with hexanes/ethyl acetate
出典と根拠
- ORDレコード
- ord-6ab3e58b2d5844cf904791881b1e8bb0
- 出典データセット
- uspto-grants-2010_08
- 特許番号
- US07786108B2
反応ノート
読み込み中…