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

Water → N-(2-(2-chlorophenyl)-4-oxo-1,4-dihydro-1,7-naphthyridin-6-yl)cyclopropanecarboxamide

HRID 468846
노트
인쇄 미리보기

반응식

HRID 468846 반응식
Cl[C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][N:11]=1)[NH:8][C:7]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[Cl:18])=[CH:6][C:5]2=[O:19].[CH:20]1([C:23]([NH2:25])=[O:24])[CH2:22][CH2:21]1.C(=O)([O-])[O-].[Cs+].[Cs+].O>O1CCOCC1.[Cl-].[Na+].O>[Cl:18][C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=1[C:7]1[NH:8][C:9]2[C:4]([C:5](=[O:19])[CH:6]=1)=[CH:3][C:2]([NH:25][C:23]([CH:20]1[CH2:22][CH2:21]1)=[O:24])=[N:11][CH:10]=2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 962WaterHCID 10796Cesium carbonateHCID 80376Cyclopropanecarboxamide2회HCID 866749476-chloro-2-(2-chlorophenyl)-1,7-naphthyridin-4(1H)-one

생성물 1

HCID 67977259N-(2-(2-chlorophenyl)-4-oxo-1,4-dihydro-1,7-naphthyridin-6-yl)cyclopropanecarboxamide수율 6.2%

시약·촉매·용매 2

HCID 31275
1,4-Dioxane
용매
HCID 57417360Sodium chloride; water용매

실험 절차

A mixture of 6-chloro-2-(2-chlorophenyl)-1,7-naphthyridin-4(1H)-one (29.2 mg, 100 μmol), cyclopropanecarboxamide (17.1 mg, 200 μmol), chloro[2-(dicyclohexylphosphino)-3,6-dimethoxy-2′-4′-6′-tri-1-propyl-1,1′-biphenyl][2-(2-aminoeth yl)phenyl]palladium(II) (8.0 mg, 10 μmol), 2-(dicyclohexylphosphino)-3,6-dimethoxy-2′-4′-6′-tri-1-propyl-1,1′-biphenyl (5.4 mg, 10 μmol), and cesium carbonate (98.0 mg, 301 μmol) in 1,4-dioxane (5.0 mL) was heated to reflux for 4 hours. Further portions of cyclopropanecarboxamide (17.1 mg, 200 μmol), chloro[2-(dicyclohexylphosphino)-3,6-dimethoxy-2′-4′-6′-tri-1-propyl-1,1′-biphenyl][2-(2-aminoeth yl)phenyl]palladium(II) (8.0 mg, 10 μmol) and 2-(dicyclohexylphosphino)-3,6-dimethoxy-2′-4′-6′-tri-1-propyl-1,1′-biphenyl (5.4 mg, 10 μmol) were added and the mixture heated to reflux for 16 hours. The cooled mixture was treated with water and brine and extracted with ethyl acetate, and the separated organic phase washed with brine, dried over sodium sulfate, filtered, and concentrated in vacuo. The residue was purified by reverse phase HPLC (gradient of acetonitrile in water with 0.1% formic acid) to afford the title compound as a white solid (2.1 mg, 6.2%). LCMS (Method E): RT=3.715 min, M+H+=340.0 & 342.0.

후처리

  1. temperaturewas heated
  2. temperatureto reflux for 4 hours
  3. temperaturethe mixture heated
  4. temperatureto reflux for 16 hours
  5. extractionextracted with ethyl acetate
  6. washthe separated organic phase washed with brine
  7. dry with materialdried over sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo
  10. customThe residue was purified by reverse phase HPLC (gradient of acetonitrile in water with 0.1% formic acid)

출처 및 근거

ORD 기록
ord-ec2c039f7a5f43f89bb96ebc222bfb74
출처 데이터셋
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08623889B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트