1-Fluoro-4-hydroxy-1,4-diazoniabicyclo[2.2.2]octane bis(tetrafluoroborate) → 5-Tert-butyl-2-fluoro-indan-1-one

HRID 451612

반응식

HRID 451612 반응식
[C:1]([C:5]1[CH:6]=[C:7]2[C:11](=[CH:12][CH:13]=1)[C:10](=[O:14])[CH2:9][CH2:8]2)([CH3:4])([CH3:3])[CH3:2].[B-](F)(F)(F)[F:16].[B-](F)(F)(F)F.C1[N+]2(O)CC[N+](F)(CC2)C1>CO>[C:1]([C:5]1[CH:6]=[C:7]2[C:11](=[CH:12][CH:13]=1)[C:10](=[O:14])[CH:9]([F:16])[CH2:8]2)([CH3:4])([CH3:2])[CH3:3]

참가 물질

4

반응물 2

HCID 27373291-Fluoro-4-hydroxy-1,4-diazoniabicyclo[2.2.2]octane bis(tetrafluoroborate)HCID 110305765-Tert-butyl-2,3-dihydroinden-1-one

생성물 1

HCID 671882305-Tert-butyl-2-fluoro-indan-1-one

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

5-tert-butyl-indan-1-one (7.53 g, 40 mmol) was dissolved in methanol (400 ml). Accufluor (32.18 g) was added, and the reaction heated to reflux for 2 hours. After cooling and removing the solvent under vacuum, the residue was taken in methylene chloride and filtered. The filtrate was washed with water, dried with magnesium sulfate, and filtered, and the solvent removed under vacuum to give 5-tert-Butyl-2-fluoro-indan-1-one, which was used without further purification. 1H NMR (300 MHz, CDCl3) 7.73 (d, 1H), 7.48 (d, 1H), 7.45 (s, 1H), 5.18-5.35 (m, 1H), 3.54-3.65 (m, 1H), 3.12-3.29 (m, 1H), 1.36 (s, 9H). MS (CSI) m/e 224 (M+NH4)+

후처리

  1. temperaturethe reaction heated
  2. temperatureto reflux for 2 hours
  3. temperatureAfter cooling
  4. customremoving the solvent under vacuum
  5. filtrationfiltered
  6. washThe filtrate was washed with water
  7. dry with materialdried with magnesium sulfate
  8. filtrationfiltered
  9. customthe solvent removed under vacuum

출처 및 근거

ORD 기록
ord-4b0788c3764f40829af90ba225641ad4
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08487116B2

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