Hydrochloric Acid → 2-Chloro-5-ethylpyridine
反応式
O=P(Cl)(Cl)Cl.[CH2:6]([N:13](/[CH:17]=[CH:18]/[CH2:19][CH3:20])C(=O)C)[C:7]1[CH:12]=CC=CC=1.[ClH:21]>CN(C=O)C>[Cl:21][C:6]1[CH:7]=[CH:12][C:18]([CH2:19][CH3:20])=[CH:17][N:13]=1参加物
5
反応条件
- 温度
- 100 °C
実験手順
To DMF (3.8 mL) at 5° C., was added POCl3 (1.4 mL) dropwise. After 5 minutes, 62b (1 g, 4.9 mmol) was added dropwise in 2 mL of DMF. The mixture was heated to 100° C. overnight. The mixture was allowed to cool to room temperature and was added dropwise to 50 mL of 1N HCl. The solution was extracted 3 times with ethyl acetate. The combined organic layer was dried, evaporated, then purified by column chromatography (eluent: 0 to 30% EtOAc in hexane) to give 0.13 g of 62c (19% yield).
後処理
- temperatureto cool to room temperature
- extractionThe solution was extracted 3 times with ethyl acetate
- customThe combined organic layer was dried
- customevaporated
- custompurified by column chromatography (eluent: 0 to 30% EtOAc in hexane)
出典と根拠
- ORDレコード
- ord-9f22f05713af4ab084ba56ced7a2109c
- 出典データセット
- uspto-grants-2012_10
- 特許番号
- US08293729B2
反応ノート
読み込み中…