Hydrochloric Acid → Methyl cis-5-aminopiperidine-3-carboxylate dihydrochloride

HRID 383789ノート

反応式

HRID 383789 の反応式
[NH2:1][C:2]1[CH:3]=[C:4]([C:8]([O:10][CH3:11])=[O:9])[CH:5]=[N:6][CH:7]=1.[ClH:12]>CO>[ClH:12].[ClH:12].[NH2:1][C@H:2]1[CH2:7][NH:6][CH2:5][C@@H:4]([C:8]([O:10][CH3:11])=[O:9])[CH2:3]1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 1514432Methyl 5-aminopyridine-3-carboxylate

生成物 1

HCID 66659965Methyl cis-5-aminopiperidine-3-carboxylate dihydrochloride

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To the solution of methyl 5-aminopyridine-3-carboxylate (700.0 mg) in MeOH (20 ml) was added 2 M aqueous solution of HCl (7 ml). And the mixture was hydrogenated (ca. 4 atm) for 1 day in a Parr low-pressure hydrogenation apparatus with a 5 wt. % Rh on Al2O3 catalyst (451.9 mg) at 80° C. Rh on Al2O3 catalyst was filtered off and the filtrate was concentrated in vacuo. The residue was solidified from the mixed solvent of CHCl3 and MeOH to give methyl cis-5-aminopiperidine-3-carboxylate dihydrochloride as a cream-colored solid.

後処理

  1. customfor 1 day
  2. customat 80° C
  3. filtrationRh on Al2O3 catalyst was filtered off
  4. concentrationthe filtrate was concentrated in vacuo

出典と根拠

ORDレコード
ord-317c56eec4e241cf807c8ef80bd53fe9
出典データセット
uspto-grants-2013_02
特許番号
US08367690B2

反応ノート

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