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

1-Fluoro-4-hydroxy-1,4-diazoniabicyclo[2.2.2]octane bis(tetrafluoroborate) → 1-(6-Bromopyridin-2-yl)-2-fluoroethanone

HRID 385995
노트
인쇄 미리보기

반응식

HRID 385995 반응식
[Br:1][C:2]1[N:7]=[C:6]([C:8](=[O:10])[CH3:9])[CH:5]=[CH:4][CH:3]=1.[F:11][B-](F)(F)F.F[B-](F)(F)F.F[N+]12CC[N+](O)(CC1)CC2>CO>[Br:1][C:2]1[N:7]=[C:6]([C:8](=[O:10])[CH2:9][F:11])[CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 27373291-Fluoro-4-hydroxy-1,4-diazoniabicyclo[2.2.2]octane bis(tetrafluoroborate)HCID 112985782-Acetyl-6-bromopyridine

생성물 1

HCID 595262991-(6-Bromopyridin-2-yl)-2-fluoroethanone

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

1-(6-Bromopyridin-2-yl)ethanone (2 g, 10.0 mmol) and 1-fluoro-4-hydroxy-1,4-diazoniabicyclo[2.2.2]octane bis(tetrafluoroborate) (9.65 g, 15.0 mmol) were combined in MeOH (100 mL) and heated to reflux for 3 days. After cooling to room temperature, the white solid (alumina) was removed by filtration and filtrate was concentrated in vacuo. The residue was taken up in EtOAc and water and extracted with EtOAc (2×). The combined organic extracts were washed with brine, dried over MgSO4, filtered, and concentrated in vacuo. The residue was stirred in a combination of 6 N HCl and Et2O overnight. The organic phase was separated and the aqueous phase extracted with Et2O. The combined organic extracts were washed with brine, dried over MgSO4, filtered, and concentrated in vacuo. Purification of the residue by silica gel column chromatography (0-20% EtOAc-hexanes) gave the title compound as a white solid.

후처리

  1. temperatureheated
  2. temperatureto reflux for 3 days
  3. customthe white solid (alumina) was removed by filtration and filtrate
  4. concentrationwas concentrated in vacuo
  5. extractionwater and extracted with EtOAc (2×)
  6. washThe combined organic extracts were washed with brine
  7. dry with materialdried over MgSO4
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo
  10. customThe organic phase was separated
  11. extractionthe aqueous phase extracted with Et2O
  12. washThe combined organic extracts were washed with brine
  13. dry with materialdried over MgSO4
  14. filtrationfiltered
  15. concentrationconcentrated in vacuo
  16. customPurification of the residue by silica gel column chromatography (0-20% EtOAc-hexanes)

출처 및 근거

ORD 기록
ord-eb637eb3f31640b8b33a6d66c56a8fd6
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08367706B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트