4,5-Diethoxy-3-fluorophthalonitrile → 5,6-diethoxy-7-fluoro-3H-isoindol-1-ylamine

HRID 1295950노트

반응식

HRID 1295950 반응식
[CH2:1]([O:3][C:4]1[C:5]([F:17])=[C:6]([C:15]#[N:16])[C:7](=[CH:10][C:11]=1[O:12][CH2:13][CH3:14])[C:8]#[N:9])[CH3:2]>C(OCC)(=O)C.C(O)C.CO.[Pt]=O>[CH2:1]([O:3][C:4]1[C:5]([F:17])=[C:6]2[C:7](=[CH:10][C:11]=1[O:12][CH2:13][CH3:14])[CH2:8][N:9]=[C:15]2[NH2:16])[CH3:2]

참가 물질

4

반응물 1

HCID 229298414,5-Diethoxy-3-fluorophthalonitrile

생성물 1

HCID 99917775,6-diethoxy-7-fluoro-3H-isoindol-1-ylamine수율 20%

시약·촉매·용매 2

HCID 82844Platinum oxide (PtO)촉매HCID 18423184Ethyl acetate ethanol methanol용매

실험 절차

After dissolving 4,5-diethoxy-3-fluorophthalonitrile (103 g) in ethyl acetate-ethanol-methanol (600 ml-600 ml-300 ml), platinum oxide (8 g) was added and the mixture was stirred at room temperature for 4 days under a hydrogen stream. The reaction mixture was filtered through celite, the organic layer was distilled off under reduced pressure and the residue was purified by silica gel column chromatography (solvent: n-hexane-ethyl acetate) to yield the title compound (21 g) as yellow crystals.

후처리

  1. additionwas added
  2. filtrationThe reaction mixture was filtered through celite
  3. distillationthe organic layer was distilled off under reduced pressure
  4. customthe residue was purified by silica gel column chromatography (solvent: n-hexane-ethyl acetate)

출처 및 근거

ORD 기록
ord-3313e0d14f764dacad535d9e1fede670
출처 데이터셋
uspto-grants-2007_07
특허 번호
US07244730B2

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