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

Sodium Hydroxide → 4-(1H-1,2,4-triazol-1-yl)benzamide

HRID 587827
노트
인쇄 미리보기

반응식

HRID 587827 반응식
BrC1C=C(C(F)(C(F)(F)F)C(F)(F)F)C=C(Br)C=1[NH2:4].[N:20]1([C:25]2[CH:33]=[CH:32][C:28]([C:29](Cl)=[O:30])=[CH:27][CH:26]=2)[CH:24]=[N:23][CH:22]=[N:21]1.[OH-].[Na+]>N1C=CC=CC=1.O.O1CCCC1>[N:20]1([C:25]2[CH:33]=[CH:32][C:28]([C:29]([NH2:4])=[O:30])=[CH:27][CH:26]=2)[CH:24]=[N:23][CH:22]=[N:21]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 14798Sodium HydroxideHCID 103198952,6-Dibromo-4-(1,1,1,2,3,3,3-heptafluoropropan-2-yl)anilineHCID 450819094-(1H-1,2,4-Triazol-1-yl)benzoyl chloride

생성물 1

HCID 219505584-(1H-1,2,4-triazol-1-yl)benzamide수율 89%

시약·촉매·용매 3

HCID 962Water용매2회
HCID 1049
Pyridine
용매
HCID 8028Tetrahydrofuran용매

실험 절차

2,6-Dibromo-4-(1,1,1,2,3,3,3-heptafluoropropan-2-yl)aniline (0.45 g) was dissolved in pyridine (5 ml). To the solution, the crude product of 4-(1H-1,2,4-triazol-1-yl)benzoyl chloride (0.45 g) was added and the mixture was refluxed under heating for 1.5 hours. After cooling to room temperature, the reaction solution was diluted with water and extracted twice with ethyl acetate. The organic phases were combined, washed with 2N hydrochloric acid and dried over magnesium sulfate. After filtering off the drying agent, the solvent was distilled off under reduced pressure to obtain a residue, which were then dissolved in tetrahydrofuran (20 ml), added with a 2N sodium hydroxide solution (5 ml) and stirred under heating at 50° C. for 2 hours. After cooling to room temperature, the reaction solution was diluted with water and extracted twice with ethyl acetate. The organic phases were combined, washed with water and dried over magnesium sulfate. After filtering off the drying agent, the solvent was distilled off under reduced pressure to obtain a crude product. The crude product was purified by column chromatography to obtain N-[2,6-d]bromo-4-(1,1,1,2,3,3,3-heptafluoropropan-2-yl)phenyl]-4-(1H-1,2,4-triazol-1-yl)benzamide (0.18 g, yield 28%).

후처리

  1. temperaturethe mixture was refluxed
  2. temperatureunder heating for 1.5 hours
  3. extractionextracted twice with ethyl acetate
  4. washwashed with 2N hydrochloric acid
  5. dry with materialdried over magnesium sulfate
  6. filtrationAfter filtering off the drying agent
  7. distillationthe solvent was distilled off under reduced pressure
  8. customto obtain a residue, which
  9. temperatureunder heating at 50° C. for 2 hours
  10. temperatureAfter cooling to room temperature
  11. extractionextracted twice with ethyl acetate
  12. washwashed with water
  13. dry with materialdried over magnesium sulfate
  14. filtrationAfter filtering off the drying agent
  15. distillationthe solvent was distilled off under reduced pressure
  16. customto obtain a crude product
  17. customThe crude product was purified by column chromatography

출처 및 근거

ORD 기록
ord-551b944f0d004f0598bb772b655bf9aa
출처 데이터셋
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09227923B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트