Dimethyl acetylenedicarboxylate → HCID 178499652、化合物
反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[NH:9][C:10]([NH2:12])=[S:11].[C:13]([C:19](OC)=[O:20])#[C:14][C:15]([O:17][CH3:18])=[O:16]>CO>[CH3:18][O:17][C:15](=[O:16])[CH:14]=[C:13]1[S:11][C:10]([NH:9][C:3]2[C:2]([Cl:1])=[CH:7][CH:6]=[CH:5][C:4]=2[Cl:8])=[N:12][C:19]1=[O:20]参加物
4
反応条件
- 温度
- 25 °C
実験手順
2,6-Dichlorophenylthiourea (3.0 g, 13.6 mmol) was dissolved in 50 mL of dry methanol and dimethyl acetylenedicarboxylate (13.8 mmol, 1.7 mL) was added over a 10-minute period. The mixture was stirred at 25° C. for 40 minutes, then the mixture was heated at 55° C. for 3 hours. The solvent was removed by rotvap, and the crude product was recrystallized from methanol to yield the desired product.
後処理
- temperaturethe mixture was heated at 55° C. for 3 hours
- customThe solvent was removed by rotvap
- customthe crude product was recrystallized from methanol
出典と根拠
- ORDレコード
- ord-47ab7d127d864fd887dbef69ec9c27e4
- 出典データセット
- uspto-grants-2003_10
- 特許番号
- US06632831B2
反応ノート
読み込み中…