Stannous Chloride → 4-Chloro-3,5-difluorobenzene-1,2-diamine
반응식
[Cl:1][C:2]1[C:3]([F:13])=[C:4]([C:6]([N+:10]([O-])=O)=[CH:7][C:8]=1[F:9])[NH2:5].Cl[Sn]Cl>C(O)C>[Cl:1][C:2]1[C:8]([F:9])=[CH:7][C:6]([NH2:10])=[C:4]([NH2:5])[C:3]=1[F:13]참가 물질
4
실험 절차
A solution of 348 mg (1.67 mmol) of 3-chloro-2,4-difluoro-6-nitroaniline and 1.57 g (8.28 mmol) of SnCl2 in 8 mL of ethanol was heated at 70° C. for 2 h. The solution was evaporated to remove the ethanol. The residue was treated with 2N NaOH to pH=13. White precipitate was observed. The mixture was extracted with CHCl3 (3×10 mL). The extract was dried (MgSO4) and evaporated to leave a red solid (285 mg, 95%); mp 77-78° C; 1H NMR (CDCl3), 3.156 (b, 2), 3.704 (b, 2), 6.352 (dd, 1, J=1.86, 9.95).
후처리
- customThe solution was evaporated
- customto remove the ethanol
- additionThe residue was treated with 2N NaOH to pH=13
- extractionThe mixture was extracted with CHCl3 (3×10 mL)
- dry with materialThe extract was dried (MgSO4)
- customevaporated
출처 및 근거
- ORD 기록
- ord-6eded7c06a29413d97ee09fc441bbde3
- 출처 데이터셋
- uspto-grants-2001_06
- 특허 번호
- US06251903B1
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