反応式
[C:1]([CH2:3][C:4]([NH:6][C:7]1[CH:12]=[C:11]([O:13][CH3:14])[C:10]([Cl:15])=[CH:9][C:8]=1[Cl:16])=[O:5])#[N:2].[NH2:17][C:18]1[CH:22]=[CH:21][S:20][CH:19]=1.[CH2:23](OC(OCC)OCC)C>C(O)(C)C>[C:1]([C:3](=[CH:23][NH:17][C:18]1[CH:22]=[CH:21][S:20][CH:19]=1)[C:4]([NH:6][C:7]1[CH:12]=[C:11]([O:13][CH3:14])[C:10]([Cl:15])=[CH:9][C:8]=1[Cl:16])=[O:5])#[N:2]参加物
実験手順
To a suspension of 2-cyano-N-(2,4-dichloro-5-methoxyphenyl)acetamide (1.57 g, 6.06 mmol) in 200 mL of iso-propanol was added 3-aminothiophene (600 mg, 6.06 mmol). This mixture was heated to reflux and triethylorthoformate (6.5 mL, 39.1 mmol) was added dropwise. The reaction mixture was heated at reflux overnight. Additional 3-aminothiophene (214 mg, 2.16 mmol) was added and the reaction mixture was heated at reflux for 5 hours. Additional 3-aminothiophene (100 mg, 1.01 mmol) was added and the reaction mixture was heated at reflux for 2.5 hours. The mixture was allowed to cool to room temperature and the solid was collected by filtration, washed with iso-propanol to give 572 mg (26%) of 2-cyano-N-(2,4-dichloro-5-methoxyphenyl)-3-(thien-3-ylamino)prop-2-enamide as a tan solid, mp >250° C.; MS 366.0, 368.2 (M−H)−
後処理
- temperatureThis mixture was heated
- temperatureto reflux
- temperatureThe reaction mixture was heated
- temperatureat reflux overnight
- temperaturethe reaction mixture was heated
- temperatureat reflux for 5 hours
- temperaturethe reaction mixture was heated
- temperatureat reflux for 2.5 hours
- filtrationthe solid was collected by filtration
- washwashed with iso-propanol
出典と根拠
- ORDレコード
- ord-5a886353dd1545818b1b995b5618d85a
- 出典データセット
- uspto-grants-2007_11
- 特許番号
- US07297795B2
関連ノート
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