Sodium Hydroxide → 1-(Pyridin-2-yl)piperidine-4-carboxylic acid

HRID 6910ノート

反応式

HRID 6910 の反応式
[OH-].[Na+].C([O:5][C:6]([CH:8]1[CH2:13][CH2:12][N:11]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][N:15]=2)[CH2:10][CH2:9]1)=[O:7])C>O1CCOCC1>[N:11]1([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][N:15]=2)[CH2:12][CH2:13][CH:8]([C:6]([OH:7])=[O:5])[CH2:9][CH2:10]1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 3815618Ethyl 1-(pyridin-2-yl)piperidine-4-carboxylate

生成物 1

HCID 177503811-(Pyridin-2-yl)piperidine-4-carboxylic acid収率 89.3%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

Sodium hydroxide solution (5M, 24.8 ml, 0.12 mol) was added drop wise to a solution of 3,4,5,6-tetrahydro-2H-[1,2′]-bipyridinyl-4-carboxylic acid ethyl ester (5.8 g, 24 mmol)(see reference Farmaco, 1993, 48(10), 1439) in 1,4-dioxane (100 ml). The mixture was stirred at room temperature for 72 hours and then evaporated under reduced pressure. The residue was purified by ion exchange chromatography on Dowex® 50 WX8 resin using methanol and ammonium hydroxide solution in water as eluant (gradient from 0:0:100 to 0:5:95 to 5:5:90). The material obtained was triturated with diethyl ether to give the title compound (4.42 g).

後処理

  1. customevaporated under reduced pressure
  2. customThe residue was purified by ion exchange chromatography on Dowex® 50 WX8 resin
  3. customThe material obtained
  4. customwas triturated with diethyl ether

出典と根拠

ORDレコード
ord-c1defd81fa024523893967969113599f
出典データセット
uspto-grants-2006_08
特許番号
US07084145B2

反応ノート

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