Potassium Carbonate → 4-(Pyridin-4-ylaminomethyl)-piperidin-3-ol

HRID 1351497노트

반응식

HRID 1351497 반응식
C(OC([N:11]1[CH2:16][CH2:15][CH:14]([CH2:17][NH:18][C:19]2[C:24](Cl)=[C:23](Cl)[N:22]=[C:21](Cl)[C:20]=2Cl)[CH:13]([OH:29])[CH2:12]1)=O)C1C=CC=CC=1.C(=O)([O-])[O-].[K+].[K+]>C(O)C.[Pd]>[N:22]1[CH:21]=[CH:20][C:19]([NH:18][CH2:17][CH:14]2[CH2:15][CH2:16][NH:11][CH2:12][CH:13]2[OH:29])=[CH:24][CH:23]=1

참가 물질

5

반응물 2

HCID 11430Potassium CarbonateHCID 235772743-Hydroxy-4-[(2,3,5,6-tetrachloro-pyridin-4-ylamino)-methyl]-piperidine-1-carboxylic acid benzyl ester

생성물 1

HCID 221356624-(Pyridin-4-ylaminomethyl)-piperidin-3-ol

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

A suspension of 3-hydroxy-4-[(2,3,5,6-tetrachloro-pyridin-4-ylamino)-methyl]-piperidine-1-carboxylic acid benzyl ester compound from Step 1 above (1.64 g) and potassium carbonate (6 g) in ethanol (200 mL) was hydrogenated at 60 psi over 1 g of 10% palladium on charcoal for 5 h. The reaction mixture was filtered and the solids washed well with ethanol. The filtrate was evaporated, taken up in 40% MeOH DCM and refiltered. The filtrate was evaporated to give crude 4-(pyridin-4-ylaminomethyl)-piperidin-3-ol product used without further purification in the next step.

후처리

  1. filtrationThe reaction mixture was filtered
  2. washthe solids washed well with ethanol
  3. customThe filtrate was evaporated
  4. customThe filtrate was evaporated

출처 및 근거

ORD 기록
ord-0a8bf320d7844f968f0fce4b0f2320b6
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07217716B2

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