Ammonia → 6-methyl-6,7-dihydro-5H-thieno[3,2-c]pyridin-4-one
反応式
[N:1]([CH:4]([CH3:11])[CH2:5][C:6]1[S:7][CH:8]=[CH:9][CH:10]=1)=[C:2]=[O:3].N>C(Cl)Cl>[CH3:11][CH:4]1[NH:1][C:2](=[O:3])[C:10]2[CH:9]=[CH:8][S:7][C:6]=2[CH2:5]1参加物
4
実験手順
To PPA (15 ml) a solution of 2-(2-isocyanatopropyl)-thiophene in CH2Cl2 (15 ml) was added. The reaction mixture was stirred under reflux for 3 h, cooled, poured into ice and alkalified with concentrated ammonia. Then, the mixture was extracted with chloroform, dried over Na2SO4 and concentrated on rotary evaporator. The residue was purified by flash column chromatography on silica gel (eluent: chloroform/acetone—0→30%) to give 0.5 g of the target compound as a white solid.
後処理
- temperatureunder reflux for 3 h
- temperaturecooled
- additionpoured into ice
- extractionThen, the mixture was extracted with chloroform
- dry with materialdried over Na2SO4
- concentrationconcentrated on rotary evaporator
- customThe residue was purified by flash column chromatography on silica gel (eluent: chloroform/acetone—0→30%)
出典と根拠
- ORDレコード
- ord-0b432daef3bb455abcf65a68ee96d7bd
- 出典データセット
- uspto-grants-2011_05
- 特許番号
- US07947689B2
反応ノート
読み込み中…