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 47533노트

반응식

HRID 47533 반응식
[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

참가 물질

5

반응물 2

HCID 178310772-[1-(1-Methoxycarbonylpiperidin-4-yl)-piperidin-4-yl]amino-3-nitropyridineHCID 178418361HCID 178418361, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-3c753ad01d3a4689adf159fe655e9a2f
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06699880B1

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