Acetic Acid → 2-chloro-3-(1H-pyrrol-1-yl)pyridine
反応式
C(O)(=O)C.[Cl:5][C:6]1[C:11]([NH2:12])=[CH:10][CH:9]=[CH:8][N:7]=1.CO[CH:15]1[CH2:19][CH2:18][CH:17](OC)O1>O>[Cl:5][C:6]1[C:11]([N:12]2[CH:15]=[CH:19][CH:18]=[CH:17]2)=[CH:10][CH:9]=[CH:8][N:7]=1参加物
5
実験手順
To 30 ml of acetic acid were added 5.0 g of 2-chloro-3-pyridinylamine and 5.6 g of 2,5-dimethoxytetrahydrofuran, and the mixture was heated to reflux for 2 hours. The reaction mixture was allowed to cool to room temperature, poured into water, and then extracted with ethyl acetate two times. The organic layers were combined, washed successively with water and an aqueous saturated sodium chloride solution, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The resulting residue was subjected to silica gel chromatography to obtain 6.5 g of 1-(2-chloro-3-pyridinyl)-1H-pyrrole of the formula:
後処理
- temperaturethe mixture was heated
- temperatureto reflux for 2 hours
- extractionextracted with ethyl acetate two times
- washwashed successively with water
- dry with materialan aqueous saturated sodium chloride solution, dried over anhydrous sodium sulfate
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-55f8504b34564a6d9ffacbca3b10db52
- 出典データセット
- uspto-grants-2011_06
- 特許番号
- US07968573B2
反応ノート
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