Hydrochloric Acid → (2,6-Dichloro-5-fluoropyridin-3-yl)methanamine

HRID 40135

反応式

HRID 40135 の反応式
Cl.[Cl:2][C:3]1[N:10]=[C:9]([Cl:11])[C:8]([F:12])=[CH:7][C:4]=1[C:5]#[N:6]>CO.[Pd]>[Cl:2][C:3]1[C:4]([CH2:5][NH2:6])=[CH:7][C:8]([F:12])=[C:9]([Cl:11])[N:10]=1

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 27338492,6-Dichloro-5-fluoro-3-pyridinecarbonitrile

生成物 1

HCID 55255125(2,6-Dichloro-5-fluoropyridin-3-yl)methanamine

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

To a Parr reaction bottle was added Pd—C (10%, 560 mg, 0.52 mmol), followed by 6 M HCl (50 ml) and a solution of 2,6-dichloro-5-fluoronicotinonitrile (Aldrich, 10.0 g, 52.4 mmol) in MeOH (100 ml). The mixture was placed under 50 psi H2 on a shaker type Parr apparatus for 21 h, filtered and concentrated. The crude was dissolved in EtOAc, basified with aqueous NaOH, and the layers were separated. The organic layer was washed with brine, dried over Na2SO4, and concentrated in vacuo to yield the title compound as crude light yellow oil. Used without further purification.

後処理

  1. customTo a Parr reaction bottle
  2. filtrationfiltered
  3. concentrationconcentrated
  4. dissolutionThe crude was dissolved in EtOAc
  5. customthe layers were separated
  6. washThe organic layer was washed with brine
  7. dry with materialdried over Na2SO4
  8. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-0f8b145b3d1e4d67813cc531a8167cc1
出典データセット
uspto-grants-2013_09
特許番号
US08524917B2

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