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HCID 68682086、化合物 → 2-Pyridinamine, 5-(1-azetidinyl)-

HRID 1952219
ノート
印刷プレビュー

反応式

HRID 1952219 の反応式
[N:1]1([C:5]2[CH:6]=[CH:7][C:8]([N+:11]([O-])=O)=[N:9][CH:10]=2)[CH2:4][CH2:3][CH2:2]1>C(O)C.[Pd]>[N:1]1([C:5]2[CH:6]=[CH:7][C:8]([NH2:11])=[N:9][CH:10]=2)[CH2:4][CH2:3][CH2:2]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 68682086HCID 68682086、化合物

生成物 1

HCID 552849632-Pyridinamine, 5-(1-azetidinyl)-

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

The 5-(azetidin-1-yl)-2-nitropyridine obtained above is taken up in 10 ml of ethanol and hydrogenated in the presence of 65 mg of 10% palladium-on-charcoal at 30° C. under a pressure of 1 bar. The reaction mixture is filtered and the filtrate is diluted with 7N ammoniacal methanol and then concentrated to dryness at 30° C. under reduced pressure. The residue is taken up in dichloromethane, an insoluble material is removed and the residue obtained after evaporation to dryness is chromatographed on a silica cartridge, elution being carried out with a mixture of dichloromethane and 7N ammoniacal methanol (90/10). The fractions comprising the expected product are combined and concentrated to give 185 mg of 5-(azetidin-1-yl)pyridine-2-amine in the form of a red oil.

後処理

  1. filtrationThe reaction mixture is filtered
  2. additionthe filtrate is diluted with 7N ammoniacal methanol
  3. concentrationconcentrated to dryness at 30° C. under reduced pressure
  4. customan insoluble material is removed
  5. customthe residue obtained
  6. customafter evaporation to dryness
  7. customis chromatographed on a silica cartridge, elution
  8. additionbeing carried out with a mixture of dichloromethane and 7N ammoniacal methanol (90/10)
  9. concentrationconcentrated

出典と根拠

ORDレコード
ord-28545cd8df344a98a8c591fe2fb04ace
出典データセット
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08404848B2

反応ノート

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