4-Chloropyridine → tert-Butyl [1-(pyridin-4-yl)piperidin-4-yl]carbamate

HRID 33241

반응식

HRID 33241 반응식
[C:1]([O:5][C:6](=[O:14])[NH:7][CH:8]1[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1)([CH3:4])([CH3:3])[CH3:2].Cl[C:16]1[CH:21]=[CH:20][N:19]=[CH:18][CH:17]=1>C(O)CCC.O.CCN(CC)CC.C(Cl)Cl>[C:1]([O:5][C:6](=[O:14])[NH:7][CH:8]1[CH2:13][CH2:12][N:11]([C:16]2[CH:21]=[CH:20][N:19]=[CH:18][CH:17]=2)[CH2:10][CH2:9]1)([CH3:4])([CH3:2])[CH3:3]

참가 물질

5

반응물 2

HCID 122884-ChloropyridineHCID 7238334-(N-Boc-amino)piperidine

생성물 1

HCID 18008972tert-Butyl [1-(pyridin-4-yl)piperidin-4-yl]carbamate

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 86625244n-butanol water NEt3용매

실험 절차

A solution of 3 g Piperidin-4-yl-carbamic acid tert-butyl ester and 2.5 g 4-Chloropyridine in 9 ml n-butanol/water/NEt3 1:1:1 was heated at 100° C. for 48 h. Then the solution was cooled to RT diluted with DCM and washed with NaHCO3 solution and water. The organic layer was dried over Na2SO4, filtered, and the solvent was removed under reduced pressure. Chromatographic purification of the residue on silica with DCM as eluent gave after evaporation of the fractions containing the product a white foam. Yield 1.7 g.

후처리

  1. washwashed with NaHCO3 solution and water
  2. dry with materialThe organic layer was dried over Na2SO4
  3. filtrationfiltered
  4. customthe solvent was removed under reduced pressure
  5. customChromatographic purification of the residue on silica with DCM as eluent
  6. customgave
  7. customafter evaporation of the fractions
  8. additioncontaining the product a white foam

출처 및 근거

ORD 기록
ord-67cb0225ae7f4dc89bfb109598d6f565
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07429581B2

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