Methyl iodide → 7-Bromo-2-methyl-1,6-naphthyridine
反応式
[NH2:1][C:2]1[CH:7]=[C:6]([Br:8])[N:5]=[CH:4][C:3]=1/[CH:9]=[CH:10]/[C:11](=O)[CH3:12].C[S-].[Na+].IC>C(O)C>[Br:8][C:6]1[CH:7]=[C:2]2[C:3]([CH:9]=[CH:10][C:11]([CH3:12])=[N:1]2)=[CH:4][N:5]=1参加物
5
実験手順
(E)-4-(4-Amino-6-bromopyridin-3-yl)but-3-en-2-one (Preparation 66, 331 mg 1.37 mmol) and sodium thiomethoxide (97.5 mg 1.39 mmol) were stirred in ethanol (2.9 mL) at 20° C. for 50 minutes. Iodomethane (86 uL, 1.38 mmole) was added and the reaction stirred for another 45 minutes. The reaction was concentrated in vacuo and diluted with ethyl acetate (30 mL) and washed with water (10 mL). The aqueous was back extracted with ethyl acetate (5 mL) and the combined organic layers were washed with brine, dried over sodium sulfate and concentrated in vacuo to afford the title compound (275 mg, 89%).
後処理
- concentrationThe reaction was concentrated in vacuo
- additiondiluted with ethyl acetate (30 mL)
- washwashed with water (10 mL)
- extractionThe aqueous was back extracted with ethyl acetate (5 mL)
- washthe combined organic layers were washed with brine
- dry with materialdried over sodium sulfate
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-77f27829e73446deb99cc615115187ac
- 出典データセット
- uspto-grants-2016_05
- 特許番号
- US09334286B2
反応ノート
読み込み中…