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5-[2-(4-Methoxybenzylamino)pyridin-6-yl]pentanoic acid ethyl ester → 5-(2-Aminopyridin-6-yl)pentanoic acid ethyl ester

HRID 2187397
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반응식

HRID 2187397 반응식
[CH2:1]([O:3][C:4](=[O:25])[CH2:5][CH2:6][CH2:7][CH2:8][C:9]1[N:14]=[C:13]([NH:15]CC2C=CC(OC)=CC=2)[CH:12]=[CH:11][CH:10]=1)[CH3:2]>C(O)(C(F)(F)F)=O>[CH2:1]([O:3][C:4](=[O:25])[CH2:5][CH2:6][CH2:7][CH2:8][C:9]1[N:14]=[C:13]([NH2:15])[CH:12]=[CH:11][CH:10]=1)[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 700925705-[2-(4-Methoxybenzylamino)pyridin-6-yl]pentanoic acid ethyl ester

생성물 1

HCID 542733055-(2-Aminopyridin-6-yl)pentanoic acid ethyl ester

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

The ester 16-3 (5.7 g) in TFA (75 mL) was heated at 60° C. for 2 hours then cooled and the excess TFA removed in vacuo. The residue was diluted with water, made basic with NaHCO3 and extracted with ether (3×). After washing the ether layer with saturated NaHCO3 then brine, it was dried (Na2SO4) and concentrated to give a viscous oil. Purification by silica gel chromatography (hexane:EtOAc 3:7) afforded the title compound 16-4 as an oil.

후처리

  1. temperaturethen cooled
  2. customthe excess TFA removed in vacuo
이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트
  • additionThe residue was diluted with water
  • extractionextracted with ether (3×)
  • washAfter washing the ether layer with saturated NaHCO3
  • dry with materialbrine, it was dried (Na2SO4)
  • concentrationconcentrated
  • customto give a viscous oil
  • customPurification by silica gel chromatography (hexane:EtOAc 3:7)
  • 출처 및 근거

    ORD 기록
    ord-647a2e460d0d41509e547cc9ac4adff4
    출처 데이터셋
    uspto-grants-2002_06
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US06410526B1

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