Methyl cyanoacetate → Methyl 2-amino-3-thenoate
反応式
[C:1]([CH2:3][C:4]([O:6][CH3:7])=[O:5])#[N:2].[S:8]1CC(O)S[CH2:10][CH:9]1O.C(N(CC)CC)C>CCO>[NH2:2][C:1]1[S:8][CH:9]=[CH:10][C:3]=1[C:4]([O:6][CH3:7])=[O:5]参加物
5
反応条件
- 温度
- 40 °C
実験手順
A mixture of methyl cyanoacetate (3.25 g, 32.3 mmol), 1,4dithiane-2,5diol (5 g, 32.8 mmol), triethylamine (1 mL, 7.71 mmol) in EtOH (50 mL) is stirred at 40° C. for 1 h. The cooled solution is eluted through a silica plug with CH2Cl2 . The filtrate is stripped to dryness to give crude methyl 2-aminothiophene-3-carboxylate which is carried on to the next reaction. 1H NMR (DMSO) δ 7.26 (1H, s), 6.82 (1H, d, J=5.8 Hz), 6.28 (1H, d, J=5.8 Hz), 3.69 (3H, s)
後処理
- washThe cooled solution is eluted through a silica plug with CH2Cl2
出典と根拠
- ORDレコード
- ord-9e33778dcd6f4845ad31802b468b952e
- 出典データセット
- uspto-grants-2004_03
- 特許番号
- US06713484B2
反応ノート
読み込み中…