반응식
[F:1][C:2]([F:7])([F:6])[CH2:3][NH:4][NH2:5].[C:8](O)(=[O:15])/[C:9](=[C:11](\[CH:13]=O)/[Cl:12])/[Cl:10]>C(O)C>[F:1][C:2]([F:7])([F:6])[CH2:3][N:4]1[C:8](=[O:15])[C:9]([Cl:10])=[C:11]([Cl:12])[CH:13]=[N:5]1참가 물질
4
실험 절차
2,2,2-Trifluoroethylhydrazine (70% solution in water, 35.0 g, 0.307 mol) was treated with mucochloric acid (51.88 g, 0.307 mol) in ethanol (300 mL) and refluxed for 5 hours. The solvent was concentrated in vacuo. The crystals obtained were washed with water and air dried (yield: 50 g; 67.5%). 1H NMR (300 MHz, CDCl3) δ 4.8 (q, J=9 Hz, 2H), 7.85 (s, 1H). MS (DCl-NH3) m/z 264 (M+NH4)+.
후처리
- temperaturerefluxed for 5 hours
- concentrationThe solvent was concentrated in vacuo
- customThe crystals obtained
- washwere washed with water and air
- customdried (yield: 50 g; 67.5%)
출처 및 근거
- ORD 기록
- ord-b275da0cabc342c7b5e85ec7bdd06e4d
- 출처 데이터셋
- uspto-grants-2001_10
- 특허 번호
- US06307047B1
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