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

4-Vinylpyridine → 3-nitro-2-[3-[(E)-2-(4-pyridyl)vinyl]phenylamino]pyridine

HRID 2086792
노트
인쇄 미리보기

반응식

HRID 2086792 반응식
I[C:2]1[CH:3]=[C:4]([NH:8][C:9]2[C:14]([N+:15]([O-:17])=[O:16])=[CH:13][CH:12]=[CH:11][N:10]=2)[CH:5]=[CH:6][CH:7]=1.[CH:18]([C:20]1[CH:25]=[CH:24][N:23]=[CH:22][CH:21]=1)=[CH2:19].C(=O)(O)[O-].[Na+]>[Cl-].C([N+](CCCC)(CCCC)CCCC)CCC.CN(C)C=O.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[N+:15]([C:14]1[C:9]([NH:8][C:4]2[CH:5]=[CH:6][CH:7]=[C:2](/[CH:19]=[CH:18]/[C:20]3[CH:25]=[CH:24][N:23]=[CH:22][CH:21]=3)[CH:3]=2)=[N:10][CH:11]=[CH:12][CH:13]=1)([O-:17])=[O:16]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 75024-VinylpyridineHCID 516892Sodium Bicarbonate2회HCID 227244832-(3-Iodophenylamino)-3-nitropyridine

생성물 1

HCID 227240493-nitro-2-[3-[(E)-2-(4-pyridyl)vinyl]phenylamino]pyridine수율 39.1%

시약·촉매·용매 3

HCID 70681Tetrabutylammonium Chloride촉매
HCID 167845
palladium(II) acetate
촉매
HCID 6228Dimethylformamide용매

반응 조건

온도
110 °C

실험 절차

A mixture of 2-(3-iodophenylamino)-3-nitropyridine (3.86 g), 4-vinylpyridine (1.78 g), palladium(II) acetate (80 mg), tetrabutylammonium chloride (3.14 g) and sodium bicarbonate (2.4 g) in N,N-dimethylformamide (20 ml) was stirred at 110° C. for 22 hours. Then the mixture was poured into aqueous sodium bicarbonate and extracted with ethyl acetate twice. The combined organic phase was washed with aqueous sodium bicarbonate and brine, dried over magnesium sulfate and concentrated. The residue was chromatographed on silica gel column (chloroform-methanol (50:1)) to give 3-nitro-2-[3-[(E)-2-(4-pyridyl)vinyl]phenylamino]pyridine (1.41 g) as an orange solid.

후처리

  1. extractionextracted with ethyl acetate twice
  2. washThe combined organic phase was washed with aqueous sodium bicarbonate and brine
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated
  5. customThe residue was chromatographed on silica gel column (chloroform-methanol (50:1))

출처 및 근거

ORD 기록
ord-99d04f24b4a64c26b014c367c4055df3
출처 데이터셋
uspto-grants-2004_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06727245B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트