Hydrochloric Acid → 5-Fluoro-2-hydrazinyl-3-methylpyridine
반응식
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]=1참가 물질
5
반응 조건
- 온도
- 110 °C
실험 절차
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+].
후처리
- 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
출처 및 근거
- ORD 기록
- ord-3ab58eddb3b44c46a3e49dca9bf90a08
- 출처 데이터셋
- uspto-grants-2016_04
- 특허 번호
- US09315503B2
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