6-(4-ethylpiperazin-1-yl)pyridine-3-carbonitrile → 6-(4-Ethyl-1-piperazinyl)-3-pyridinemethanamine

HRID 490084ノート

反応式

HRID 490084 の反応式
[CH2:1]([N:3]1[CH2:8][CH2:7][N:6]([C:9]2[CH:16]=[CH:15][C:12]([C:13]#[N:14])=[CH:11][N:10]=2)[CH2:5][CH2:4]1)[CH3:2].[H][H]>[Ni].CO.C(OCC)(=O)C.N>[CH2:1]([N:3]1[CH2:4][CH2:5][N:6]([C:9]2[N:10]=[CH:11][C:12]([CH2:13][NH2:14])=[CH:15][CH:16]=2)[CH2:7][CH2:8]1)[CH3:2]

参加物

7

反応物 2

HCID 167483946-(4-ethylpiperazin-1-yl)pyridine-3-carbonitrileHCID 178418361HCID 178418361、化合物

生成物 1

HCID 167882546-(4-Ethyl-1-piperazinyl)-3-pyridinemethanamine収率 103.8%

試薬・触媒・溶媒 4

HCID 935Nickel触媒HCID 222Ammonia溶媒HCID 887Methanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of 2 g (8 mmol) 6-(4-ethyl-piperazin-1-yl)-nicotinonitrile, 1.3 g Raney Nickel (B113Z, Degussa) in 25 ml methanol, 15 ml ethyl acetate and 5 ml ammonia aq. (ca. 25%) was treated with 1 bar hydrogen at 30-35° C. for 4 h. The mixture was filtered and the residue washed three times with 20 ml ethyl acetate each and the combined organic phases evaporated to dryness to yield 1.83 g (97%) of the title compound as white crystals. (m/e): 261.1 (MH+; 100%).

後処理

  1. filtrationThe mixture was filtered
  2. washthe residue washed three times with 20 ml ethyl acetate each and the combined organic phases
  3. customevaporated to dryness

出典と根拠

ORDレコード
ord-557573b2eabb4b8fa66855591abd3a0c
出典データセット
uspto-grants-2009_05
特許番号
US07528135B2

反応ノート

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