Hydrochloric Acid → 5-Fluoro-2-hydrazinyl-3-methylpyridine
反応式
C(=[N:14][NH:15][C:16]1[C:21]([CH3:22])=[CH:20][C:19]([F:23])=[CH:18][N:17]=1)(C1C=CC=CC=1)C1C=CC=CC=1.Cl>C1(C)C=CC=CC=1.O>[F:23][C:19]1[CH:20]=[C:21]([CH3:22])[C:16]([NH:15][NH2:14])=[N:17][CH:18]=1参加物
5
反応条件
- 温度
- 110 °C
実験手順
A solution of Intermediate 105a (194 mg, 0.635 mmol) in toluene (13 mL) was treated with HCl (37%, 3.5 mL) and heated at 110° C. for 1.5 h. After cooling to RT, the reaction mixture was diluted with water and extracted with toluene (×3). The aqueous layer was cooled to 0° C., neutralised with 5N NaOH and extracted with DCM (×3). The combined organic layers were dried (MgSO4) and concentrated in vacuo to afford the title compound (78 mg, 86%) as a silver/green solid. LCMS (Method 4): Rt 0.29 min, m/z 142 [MH+].
後処理
- temperatureAfter cooling to RT
- extractionextracted with toluene (×3)
- temperatureThe aqueous layer was cooled to 0° C.
- extractionextracted with DCM (×3)
- dry with materialThe combined organic layers were dried (MgSO4)
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-3ab58eddb3b44c46a3e49dca9bf90a08
- 出典データセット
- uspto-grants-2016_04
- 特許番号
- US09315503B2
反応ノート
読み込み中…