(4-Benzenesulphonyl-6-bromopyridin-2-yl)-methylamine → (4-Benzenesulphonylpyridin-2-yl)-methylamine

HRID 1603550ノート

反応式

HRID 1603550 の反応式
[C:1]1([S:7]([C:10]2[CH:15]=[C:14](Br)[N:13]=[C:12]([NH:17][CH3:18])[CH:11]=2)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1>C(O)C.[Pd]>[C:1]1([S:7]([C:10]2[CH:15]=[CH:14][N:13]=[C:12]([NH:17][CH3:18])[CH:11]=2)(=[O:9])=[O:8])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

4

反応物 1

HCID 15410397(4-Benzenesulphonyl-6-bromopyridin-2-yl)-methylamine

生成物 1

HCID 15410398(4-Benzenesulphonylpyridin-2-yl)-methylamine収率 37%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

0.09 g (0.000275 mol) of (4-benzenesulphonyl-6-bromopyridin-2-yl)-methylamine was dissolved in 7 ml of ethanol, treated with 0.009 g of Pd/C (10%) and hydrogenated under normal pressure for 18 hrs. Thereafter, the catalyst was filtered off, the solvent was removed and the residue was partitioned in ethyl acetate and saturated bicarbonate solution. The organic phase was washed with sat. sodium chloride solution and dried over MgSO4. After removal of the solvent the residue was chromatographed on silica gel with ethyl acetate/hexane 1:4 and 1:3. There was obtained 0.025 g (37%) of (4-benzenesulphonylpyridin-2-yl)-methylamine as beige crystals; m.p.: 142-143° C.

後処理

  1. filtrationThereafter, the catalyst was filtered off
  2. customthe solvent was removed
  3. customthe residue was partitioned in ethyl acetate
  4. washThe organic phase was washed with sat. sodium chloride solution
  5. dry with materialdried over MgSO4
  6. customAfter removal of the solvent the residue
  7. customwas chromatographed on silica gel with ethyl acetate/hexane 1:4 and 1:3

出典と根拠

ORDレコード
ord-512af824325540de941a68cc448b03dc
出典データセット
uspto-grants-1999_11
特許番号
US05990105

反応ノート

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