Hydrochloric Acid → 7-Fluoro-1H-pyrrolo[3,2-C]pyridine
反応式
C(O[CH:4]=[CH:5][C:6]1[CH:7]=[N:8][CH:9]=[C:10]([F:13])[C:11]=1[NH2:12])C.Cl>CCO>[F:13][C:10]1[C:11]2[NH:12][CH:4]=[CH:5][C:6]=2[CH:7]=[N:8][CH:9]=1参加物
4
実験手順
A mixture of 3-(2-ethoxy-vinyl)-5-fluoro-pyridin-4-ylamine (Preparation 63, 3.6 g, 19.2 mmol) and concentrated HCl (10 mL) in EtOH (44 mL) was heated to reflux for 4 hours before cooling and concentrating in vacuo. The residue was basified with saturated aqueous NaHCO3 solution, extracted in DCM, the organic layer collected, dried over sodium sulphate and concentrated in vacuo. The residue was purified using silica gel column chromatography eluting with 20-100% EtOAc in hexane to afford the title compound (1.7 g)
後処理
- temperaturewas heated
- temperatureto reflux for 4 hours
- temperaturebefore cooling
- concentrationconcentrating in vacuo
- extractionextracted in DCM
- customthe organic layer collected
- dry with materialdried over sodium sulphate
- concentrationconcentrated in vacuo
- customThe residue was purified
- washeluting with 20-100% EtOAc in hexane
出典と根拠
- ORDレコード
- ord-996d3db6451549c5aafd800d14c8c6ae
- 出典データセット
- uspto-grants-2015_10
- 特許番号
- US09163021B2
反応ノート
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