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Sodium Methoxide → 1-Boc-4-[(pyrid-4-ylamino)methyl]piperidine

HRID 1837494
ノート
印刷プレビュー

反応式

HRID 1837494 の反応式
[C:1]([N:8]1[CH2:13][CH2:12][CH:11]([CH2:14][NH:15][C:16]2[C:21](Cl)=[C:20](Cl)[N:19]=[C:18](Cl)[C:17]=2Cl)[CH2:10][CH2:9]1)([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].C[O-].[Na+]>CO.C1COCC1.[Pd]>[C:1]([N:8]1[CH2:9][CH2:10][CH:11]([CH2:14][NH:15][C:16]2[CH:21]=[CH:20][N:19]=[CH:18][CH:17]=2)[CH2:12][CH2:13]1)([O:3][C:4]([CH3:6])([CH3:7])[CH3:5])=[O:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 10942334Sodium MethoxideHCID 22677919HCID 22677919、化合物

生成物 1

HCID 226779521-Boc-4-[(pyrid-4-ylamino)methyl]piperidine収率 59%

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a stirred solution of 1-Boc-4-[(2,3,5,6-tetrachloropyrid-4-ylamino)methyl]piperidine (2.5 g, 5.83 mmol) in a mixture of methanol (23 mL) and THF (23 mL) was added sodium methoxide (1.89 g, 35 mmol) and 5% palladium on carbon (1.24 g). The mixture was hydrogenated for 30 h and the cataylst was filtered off and the solution concentrated in vacuo. The residue was taken up in ethyl acetate and washed with water and satd sodium bicarbonate. The aqueous washes were back extracted with ethyl acetate, and the combined organics dried (MgSO4) and concentrated in vacuo to give the product (1.0 g, 59%).

後処理

  1. filtrationthe cataylst was filtered off
  2. concentrationthe solution concentrated in vacuo
  3. washwashed with water
  4. extractionThe aqueous washes were back extracted with ethyl acetate
  5. dry with materialthe combined organics dried (MgSO4)
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-5af1fc7d32554ce3bb931c96f7a64dc0
出典データセット
uspto-grants-2004_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06784182B2

反応ノート

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