2-[1-(1-Methoxycarbonylpiperidin-4-yl)-piperidin-4-yl]amino-3-nitropyridine → 3-Amino-2-[1-(1-methoxycarbonylpiperidin-4-yl)-piperidin-4-yl]aminopyridin

HRID 47533ノート

反応式

HRID 47533 の反応式
[CH3:1][O:2][C:3]([N:5]1[CH2:10][CH2:9][CH:8]([N:11]2[CH2:16][CH2:15][CH:14]([NH:17][C:18]3[C:23]([N+:24]([O-])=O)=[CH:22][CH:21]=[CH:20][N:19]=3)[CH2:13][CH2:12]2)[CH2:7][CH2:6]1)=[O:4].[H][H]>CO.[Pd]>[NH2:24][C:23]1[C:18]([NH:17][CH:14]2[CH2:15][CH2:16][N:11]([CH:8]3[CH2:9][CH2:10][N:5]([C:3]([O:2][CH3:1])=[O:4])[CH2:6][CH2:7]3)[CH2:12][CH2:13]2)=[N:19][CH:20]=[CH:21][CH:22]=1

参加物

5

反応物 2

HCID 178310772-[1-(1-Methoxycarbonylpiperidin-4-yl)-piperidin-4-yl]amino-3-nitropyridineHCID 178418361HCID 178418361、化合物

生成物 1

HCID 227452603-Amino-2-[1-(1-methoxycarbonylpiperidin-4-yl)-piperidin-4-yl]aminopyridin

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

Seventy (70) mg of 2-[1-(1-methoxycarbonylpiperidin-4-yl)-piperidin-4-yl]amino-3-nitropyridine was dissolved in 5 ml of methanol, and to which 20 mg of 10% palladium/carbon catalyst was added to effect catalytic reduction at room temperature under atmospheric pressure of hydrogen. After filtering the catalyst off and drying the filtrate to solid, the resulting residue was purified by silica gel column chromatography (chloroform/methanol=95/5) to give 20 mg of 3-amino-2-[1-(1-methoxycarbonylpiperidin-4-yl)-piperidin-4-yl]aminopyridin.

後処理

  1. customat room temperature
  2. filtrationAfter filtering the catalyst off and
  3. customdrying the filtrate to solid
  4. customthe resulting residue was purified by silica gel column chromatography (chloroform/methanol=95/5)

出典と根拠

ORDレコード
ord-3c753ad01d3a4689adf159fe655e9a2f
出典データセット
uspto-grants-2004_03
特許番号
US06699880B1

反応ノート

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