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

Monobasic potassium phosphate → 4-Fluoro-3-nitropyridine

HRID 34269
노트
인쇄 미리보기

반응식

HRID 34269 반응식
[F-:1].[K+].Cl[C:4]1[CH:9]=[CH:8][N:7]=[CH:6][C:5]=1[N+:10]([O-:12])=[O:11].P([O-])(O)(O)=O.[K+]>CS(C)=O>[F:1][C:4]1[CH:9]=[CH:8][N:7]=[CH:6][C:5]=1[N+:10]([O-:12])=[O:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 516951Monobasic potassium phosphateHCID 522689Potassium FluorideHCID 27357814-Chloro-3-nitropyridine

생성물 1

HCID 201291284-Fluoro-3-nitropyridine수율 52%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

Anhydrous potassium fluoride (5.5 g, 93 mmol) was suspended in anhydrous dimethylsulfoxide (200 ml) and the solvent reduced to half its volume by distillation under an atmosphere of nitrogen. The resulting suspension was cooled to room temperature and 4-chloro-3-nitropyridine (14 g, 88 mmol) was added. The reaction mixture was stirred at 120° C. for three hours under an atmosphere of nitrogen, cooled and then poured into a saturated aqueous solution of potassium dihydrogen phosphate. The resulting mixture was extracted with ethyl acetate. The organic phase was washed three times with water and then brine before being dried over anhydrous magnesium sulphate. The solvent was removed in vacuo to yield as an oil, 4-fluoro-3-nitropyridine (6.5 g), (δ(CDCl3) 7.32 (1H, 4 lines), 7.86 (1H, t, J=5 Hz) and 8.29 (1H, d, J=9 Hz), represented by the structural formula: ##STR21##

후처리

  1. distillationthe solvent reduced to half its volume by distillation under an atmosphere of nitrogen
  2. temperaturecooled
  3. extractionThe resulting mixture was extracted with ethyl acetate
  4. washThe organic phase was washed three times with water
  5. dry with materialbrine before being dried over anhydrous magnesium sulphate
  6. customThe solvent was removed in vacuo

출처 및 근거

ORD 기록
ord-0934ce69450b469a869b959ad0d0d886
출처 데이터셋
uspto-grants-1988_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04761414

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트