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

HRID 1603550노트

반응식

HRID 1603550 반응식
[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

참가 물질

4

반응물 1

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

생성물 1

HCID 15410398(4-Benzenesulphonylpyridin-2-yl)-methylamine수율 37%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-512af824325540de941a68cc448b03dc
출처 데이터셋
uspto-grants-1999_11
특허 번호
US05990105

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