Ethyl Acetate → (R)-2-(3-bromo-4-cyanophenylamino)propanamide
反応式
[Br:1][C:2]1[CH:9]=[C:8](F)[CH:7]=[CH:6][C:3]=1[C:4]#[N:5].Cl.[NH2:12][C@@H:13]([C:15]([NH2:17])=[O:16])[CH3:14].CC(N(C)C)=O.CCOC(C)=O>CS(C)=O.O>[Br:1][C:2]1[CH:9]=[C:8]([NH:12][C@H:13]([CH3:14])[C:15]([NH2:17])=[O:16])[CH:7]=[CH:6][C:3]=1[C:4]#[N:5]参加物
7
実験手順
A solution of 2-bromo-4-fluorobenzonitrile (200 mg, 1.00 mmol), D-alanine amide hydrochloride (148 mg, 1.19 mmol) and DMA (0.620 mL, 3.56 mmol) in DMSO (3 mL) was stirred at 100 C for 18 h. EtOAc and water were added. The organic phase was separated, dried over Na2SO4, concentrated in vacuo. The residue was purified by a silica gel column, eluted first with 30% EtOAc in hexane, then with 100% EtOAc to give (R)-2-(3-bromo-4-cyanophenylamino)propanamide (185 mg).
後処理
- customThe organic phase was separated
- dry with materialdried over Na2SO4
- concentrationconcentrated in vacuo
- customThe residue was purified by a silica gel column
- washeluted first with 30% EtOAc in hexane
出典と根拠
- ORDレコード
- ord-b944b628013f4510976ce132dfb416ca
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08846928B2
反応ノート
読み込み中…