Methyl 3-amino-2-thiophenecarboxylate → HCID 5178717、化合物
反応式
[CH3:1][O:2][C:3]([C:5]1[S:6][CH:7]=[CH:8][C:9]=1[NH2:10])=[O:4]>C(CC(OC)=O)#N>[CH3:1][O:2][C:3]([C:5]1[S:6][CH:7]=[CH:8][C:9]=1[NH:10][C:3](=[O:2])[CH2:5][C:9]#[N:10])=[O:4]参加物
3
実験手順
A solution of methyl-3-amino-thiophene-2-carboxylate (13 g, 82.70 mmol) in neat methyl cyanoacetate (40 mL) was heated at 210° C. for 10 h. The solution was cooled and excess methyl cyanoacetate was distilled off under vacuum. The residue was taken in methanol, sonicated briefly, and filtered. The solids were washed by cold methanol and dried to yield 9.3 g (50%) of 3-(2-cyano-acetylamino)-thiophene-2-carboxylic acid methyl ester as white solids. MP 146° C.; 1H NMR (400 MHz, DMSO-d6) δ 4.18 (s, 2H), 7.86 (d, J=5.2 Hz, 1H), 7.93 (d, J=5.2 Hz, 1H), 10.25 (s, 1H) ppm; MS m/z=225 amu (M++1).
後処理
- temperatureThe solution was cooled
- distillationexcess methyl cyanoacetate was distilled off under vacuum
- customsonicated briefly
- filtrationfiltered
- washThe solids were washed by cold methanol
- customdried
出典と根拠
- ORDレコード
- ord-d744d1e5b27446b5b3e6125be36e4561
- 出典データセット
- uspto-grants-2008_04
- 特許番号
- US07365200B2
反応ノート
読み込み中…