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

HRID 40135

반응식

HRID 40135 반응식
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

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0f8b145b3d1e4d67813cc531a8167cc1
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08524917B2

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