홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

1-Propanol → propyl 3-[3-(2-oxo-2-propoxyethyl)-1H-indol-2-yl]propanoate

HRID 476223
노트
인쇄 미리보기

반응식

HRID 476223 반응식
CS(O)(=O)=O.O=[C:7]1[N:12]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)N=[C:10](CCC(OCC)=O)[CH2:9][CH2:8]1.[OH-:26].[Na+].[CH2:28]([OH:31])[CH2:29][CH3:30]>>[O:31]=[C:28]([O:31][CH2:28][CH2:29][CH3:30])[CH2:29][C:30]1[C:14]2[C:13](=[CH:18][CH:17]=[CH:16][CH:15]=2)[NH:12][C:7]=1[CH2:8][CH2:9][C:10]([O:31][CH2:28][CH2:29][CH3:30])=[O:26]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 4

HCID 10311-PropanolHCID 6395Methanesulfonic AcidHCID 14798Sodium HydroxideHCID 21630617Ethyl 3-(6-oxo-1-phenyl-1,4,5,6-tetrahydropyridazin-3-yl)propanoate

생성물 1

HCID 59487250propyl 3-[3-(2-oxo-2-propoxyethyl)-1H-indol-2-yl]propanoate수율 79%

반응 조건

온도
80 °C

실험 절차

Methanesulfonic acid (1.15 equiv.) was added to a stirred solution of ethyl 3-(6-oxo-1-phenyl-1,4,5,6-tetrahydropyridazin-3-yl)propanoate from Step 1 in n-propanol (1.1 M). The mixture was stirred overnight at 80° C. The mixture was cooled to room temperature and neutralized with aqueous 1N NaOH (1 equiv.). Final mixture was concentrated under vacuum, diluted with toluene and concentrated again. The residue was purified by column chromatography on silica gel using automatized gradiant pump system CombiFlashRF (Teledyne ISCO) eluting with ethyl acetate/hexane (0:100 to 60:40) to give the title compound (79%) as a brown oil.

후처리

  1. concentrationFinal mixture was concentrated under vacuum
  2. additiondiluted with toluene
  3. concentrationconcentrated again
  4. customThe residue was purified by column chromatography on silica gel using automatized gradiant pump system CombiFlashRF (Teledyne ISCO)
  5. washeluting with ethyl acetate/hexane (0:100 to 60:40)

출처 및 근거

ORD 기록
ord-0b4718e0eecc4e0bb88ad95c30455e85
출처 데이터셋
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08637671B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트