반응식
[F:1][C:2]1[CH:7]=[C:6]([NH2:8])[CH:5]=[CH:4][N:3]=1.[C:9]1([N:15]=[C:16]=[O:17])[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1>C1C=CC=CC=1>[F:1][C:2]1[CH:7]=[C:6]([NH:8][C:16]([NH:15][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[O:17])[CH:5]=[CH:4][N:3]=1참가 물질
4
실험 절차
112 mg (1 mmol) of 2-fluoro-4-aminopyridine was added to 9 ml of dry benzene and to the resulting solution was further added 119 mg (1 mmol) of phenyl isocyanate. After stirring at room temperature for 30 hrs., the crystals which deposited were collected by filtration and then subjected to chromatography in a conventional manner using alumina. After developing the column with a benzene-ethyl acetate (3:1 by volume) solvent mixture, eluate containing the objective compound was collected. After distilling solvent off under reduced pressure, the residue was recrystallized from an ethyl acetate-n-hexane solvent mixture to give 113 mg of the objective compound: yield 48.9%; m.p. 179°-180° C.
후처리
- filtration, the crystals which deposited were collected by filtration
- additioneluate containing the objective compound
- customwas collected
- distillationAfter distilling solvent off under reduced pressure
- customthe residue was recrystallized from an ethyl acetate-n-hexane solvent mixture
출처 및 근거
- ORD 기록
- ord-2b870d114b884298a85da9197f8358a7
- 출처 데이터셋
- uspto-grants-1981_07
- 특허 번호
- US04279639
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