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

HRID 1827134ノート

反応式

HRID 1827134 の反応式
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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-d66e93e357cb4d2d9dae39c0fa3cbde0
出典データセット
uspto-grants-2006_05
特許番号
US07053089B2

反応ノート

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