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

HRID 1295950ノート

反応式

HRID 1295950 の反応式
[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]

参加物

4

反応物 1

HCID 229298414,5-Diethoxy-3-fluorophthalonitrile

生成物 1

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

試薬・触媒・溶媒 2

HCID 82844Platinum oxide (PtO)触媒HCID 18423184Ethyl acetate ethanol methanol溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-3313e0d14f764dacad535d9e1fede670
出典データセット
uspto-grants-2007_07
特許番号
US07244730B2

反応ノート

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