Acetic Acid → 2-Chloro-4-ethyl-5-fluoropyrimidine
反応式
[Cl:1][C:2]1[N:7]=[C:6](Cl)[C:5]([F:9])=[CH:4][N:3]=1.[C:10](O)(=O)[CH3:11]>Cl>[Cl:1][C:2]1[N:7]=[C:6]([CH2:10][CH3:11])[C:5]([F:9])=[CH:4][N:3]=1参加物
4
反応条件
- 温度
- 100 °C
実験手順
The product of part (i) (3.2 g) was dissolved in acetic acid (25 ml) and diluted with 5N HCl (10 ml). After heating the mixture at 100° C. for 16 hours the mixture was cooled and partitioned between water (30 ml) and dichloromethane (45 ml). The dichloromethane layer was separated, dried and concentrated under reduced pressure to give an oil. The title compound was isolated by chromatography on silica gel using dichloromethane as the eluent. The product was characterised by 1 H-NMR and mass spectrometry (yield=350 mg).
後処理
- temperaturewas cooled
- custompartitioned between water (30 ml) and dichloromethane (45 ml)
- customThe dichloromethane layer was separated
- customdried
- concentrationconcentrated under reduced pressure
- customto give an oil
出典と根拠
- ORDレコード
- ord-bc8c36e2106e4f47a01bbba9ec77f9ac
- 出典データセット
- uspto-grants-1998_06
- 特許番号
- US05773443
反応ノート
読み込み中…