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

HRID 6910노트

반응식

HRID 6910 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-c1defd81fa024523893967969113599f
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07084145B2

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